You are on page 1of 152

Training Manual on QUALITY ASSESSMENT OF FOOD PRODUCTS

College of Food and Dairy Technology

Tamil Nadu Veterinary and Animal Sciences University Koduvalli, Chennai - 52.

Training Manual on Quality Assessment of Food Products

151

152

Training Manual on Quality Assessment of Food Products

CONTENT
S.No. Title Chapter 1 1. 2. 3. Total Quality Management in Food Industry Advancements in Food Inspection Tools Sampling of Food Products. Chapter 2 4. 5. Quality Control of Milk and Milk Products Bacteriology of Water Chapter 3 6. 7. 8. Quality control of Meat Estimation of Egg Qualities Quality Control of Fish Chapter 4 9. 10. Fruit and Vegetables Storage Guidelines Adulterants in Foods and its Detection Methods Chapter 5 11. 12. 13. Quality Testing of Bakery Products Permissible Limit of Contaminants, Toxins and Residues in Various Food Products Procedure for Packaging of Various Food Products Chapter 6 14. 15. Food Borne Diseases Prevention and Control of Food-Borne Diseases. Page No.

Training Manual on Quality Assessment of Food Products

153

154

Training Manual on Quality Assessment of Food Products

CHAPTER 1

Training Manual on Quality Assessment of Food Products

Training Manual on Quality Assessment of Food Products

TOTAL QUALITY MANAGEMENT SYSTEMS IN FOOD INDUSTRY


G. Sujatha1, D. Baskaran2
2

Assistant Professor, College of Food and Dairy Technology, Koduvalli, Chennai 600 052 Professor and Head, Department of Food Engineering, College of Food and Dairy Technology, Koduvalli, Chennai 600 052

Quality and food safety have become competitive edge in the global market for the enterprises producing and marketing foods products. Therefore, the installation of ISO 14000, ISO 22000 Quality Management Systems and Hazard Analysis and Critical Control Points (HACCP) based food safety system is extremely desirable in view of the changing scenario of food market in the international trade. With a view to motivating the food processing industries for adoption/ implementation of food safety and quality assurance mechanisms such as Total Quality Management (TQM) including, ISO 14000, ISO 22000, HACCP, Good Manufacturing Practices (GMP), Good Hygienic Practices (GHP) and prepare them to face the global competition in post WTO era, Ministry of Food Processing Industries is implementing a Plan Scheme for Setting up/ Up-gradation of Quality Control/ Food Testing Laboratory/ R &D and Promotional Activity. The objectives of this Plan Scheme are as under 1. 2. 3. 4. 5. 6. To motivate the food processing industries for adoption of food safety and quality assurance mechanisms such as TQM including ISO 14000, ISO 22000, HACCP, GMP, GHP; To prepare them to face global competition in post WTO Regime; To enable adherence to stringent quality and hygiene norms; To enhance product acceptance by overseas buyers; To keep Indian industry technologically abreast of international best practices; To focus attention on the development of Food Processing Industries through participation, directly or indirectly, in seminar, workshop, international events etc.

The scheme has the following components


Setting Up/ Up-gradation of Quality Control/ Food Testing Laboratory Implementation of HACCP/ ISO 22000, ISO 14000/ GHP/ GMP Etc. Research & Development in the Food Processing Sector Promotional Activities

The outlay under the scheme during 11th Five year plan was Rs 250.00 crore. As against this, the Budget allocation under the scheme was of the order of Rs. 140.30 crore. Of this, the Ministry utilized Rs. 126.36 crore. TOTAL QUALITY MANAGEMENT SYSTEM Quality management is becoming increasingly important to the leadership and management of all companies for competitive advantage, thus it is important to view TQM as a distinct management

Training Manual on Quality Assessment of Food Products

philosophy which advocates of excellent management of every department of the company. Total quality management (TQM) is a management philosophy for continuously improving quality of goods and services delivered through the participation of all organizational members; it is the process of making quality the concern of every-one in the company (Zelealem & Getachew,2002). TQM mainly focuses on 1. 2. 3. 4. Customer satisfaction Human resource management Continuous improvement Leadership and management

Effective measurement of total quality cost gives the following benefits 1. 2. 3. 4. 5. increased opportunity to make objective business decisions based on quantitative data rather than judgment identification and priotization of areas and aspects of the business requiring quality improvement and quality cost reduction ability to compare the performance of departments and processes as well as in some instances the performance of the company against competitors improved quality in budgeting and cost control with the standardization of measures of performance and comparators increase in the focus of management on quality and quality improvement as an integral part of management responsibility.

TQM philosophy champions a considerable number of concepts which are fundamental for effectively quality management, are 1. Customer Focus: TQM champions customer satisfaction, thus companies should be aware of the customer quality needs and should work to achieve them in order to retain customer goodwill and maintaining the market share Quality Assurance: Food products produced should satisfy or exceed the minimum required quality standards. Furthermore products should abide to the local quality regulations as well as the international ones e.g ISO standards. Food companies use Hazard Analysis Critical Control Point (HACCP) as a quality assurance strategy. Benchmarking: The TQM philosophy highlights that companies should engage in benchmarking activities to monitor control and assess the companys products, ser-vices and processes relative to other highly performing companies. This includes product, energy, strategic, processes and financial benchmarking Maintenance: TQM highlights that adequate maintenance of the companies processes should be initiated to ensure perpetual excellence of processes. Effective organization-al maintenance is achieved through Total Productive maintenance focus office TPM, quality and planned maintenance.
Training Manual on Quality Assessment of Food Products

2.

3.

4.

5.

Human Resource management: The TQM philosophy most importantly focuses on the human resource of the company emphasis mainly on motivation and employee satisfaction through adequate salaries, training and education, empowerment and involvement in an effort to harness commitment from all employees.

Thus Total Quality Management (TQM) needs great under-standing to properly manage and achieve quality performance of any organization. The use of accounting concepts to justify investment in TQM should not be applied because the management philosophy materializes after a considerable time period. However companies and stakeholders should look at other entities to justify TQM implementation. These include

Product quality & customer satisfaction Rate of employee absenteeism Quality rate and O.E.E Scrap and rework levels Customer goodwill and market share Due date performance ISO certification success levels Accidents and health risks Market response

The Hierarchy of TQM performance indices 1. Customer Focus 2. Quality Assurance 3. Benchmarking 4. Process quality control 5. Supplier Management 6. Environmental and safety management 7. Strategic quality planning 8. Production management 9. Leadership and Management 10. Teamwork and quality circles 11. Continuous improvement 12. Maintenance 13. Employee involvement & empowerment
Training Manual on Quality Assessment of Food Products 5

14. Training and education 15. Human resource management 16. Employee satisfaction 17. Information analysis 18. Social responsibility. The results show that the food manufacturing and processing industry at the moment (2010-2011) is mainly focused on the customer. As shown by the hierarchy concepts of customer focus, quality assurance, benchmarking and process quality control are highly ranking. Furthermore concepts which mainly focus on the employee are sidelined as highlighted by the hierarchy. Employee satisfaction, human re-source planning, empowerment and involvement are low ranking. SIX SIGMA Six Sigma is a project-, data- and technology-driven quality management tool and acts as a business improvement strategy in order to improve the business competitiveness through reducing the defects and improving customer-oriented quality. Six Sigma is a highly and rigorously systematic approach to greater quality based on figures and facts and it is one of the best tools to measure the performance in an organization of any size or in any process. A food distribution SME is in the so-called service industry in which quality attribution is unlikely to be clear for the quality management team due to unclear customer assessment and customer satisfaction criteria. Therefore, Six Sigma could be a good approach, since it is a process based on performance measurement and this is a fundamental requirement to improve the Supply Chain. Arguably, Six Sigma is not always a bunch of clear and great results in the service industry. It has been suggested that implementing Six Sigma in the service industry could be more difficult in the manufacturing side, as the human recourses and ambiguity could impact on the application of Six Sigma.

Figure- complexity of food chain with food distribution in centre Six Sigma has a great link with other quality initiatives and highlights the values of the integrated approach of all these tools to achieve a collaborative Supply Chain in the food distribution SME. Six Sigma is a combination of the Six Sigma statistical metric and TQM, with additional innovations that enhance the programs effectiveness while expanding its focus. The main components of Six Sigma retained from TQM include a focus on the customer, recognition that the quality is the responsibility of
6 Training Manual on Quality Assessment of Food Products

all employees, and the emphasis on employee training. The importance of the integrated view of these quality initiatives will enable the management team in food distribution SME to avoid individualistic views and, instead, enlarge their cross-functional view and increase their ability to look at quality from different angles. It is believed that TQM is an approach to improving the competitiveness, effectiveness and flexibility of a whole organization. The impact of TQM on any organization is first to ensure that the management adopts a strategic view of quality. Six Sigma as a tail of TQM can be next step to identify the most critical aspects of quality and solve the problems through performance measurement in a systematic way. Contribution of Six Sigma in Supply Chain has been acknowledged as its methodology can be adopted to improve Supply Chain through different aspects. It has been indicated that Six Sigma has proven to be extremely valuable by reducing the cycle time, by providing new problem- solving tools and by providing improved functional and customer alignment and by allowing calculations of the value of R & D. Six Sigma has a collaborative interaction with SC as balanced score card is a top requirement for both to define the customer requirements. FISH BONE DIAGRAM The fishbone diagram, also called the Ishikawa diagram, was created in Japan. The fish bone diagrams have since become popular in many parts of the modern business world, including in manufacturing, where they can be useful in assessing what has gone wrong with a complex process. Fishbone diagrams are composed of a main horizontal line where smaller lines branch off of the main line diagonally. This makes the chart look like a fish skeleton. The fish bones represent cause and effect in a situation where its necessary to troubleshoot a production problem or other dilemma. The fishbone diagram provides a much better quick picture perspective than a block of text, which is a main part of its appeal to busy executives. Fishbone diagrams for product design, quality control, and other common uses often group different types of causal factors onto the same fish bone or category. These include people, or those who are involved in the process, as well as Method, or how the job was designed to be done. Other categories include Machines, the gear used in the process, Materials, the raw goods used, and Environment, a larger catch-all term for a variety of causal factors. Some types of fishbone diagrams use words with the same beginning letter to promote easy categorization.

Training Manual on Quality Assessment of Food Products

Fishbone diagrams could be called an aggregate model since they incorporate smaller causes contributing to larger ones. This is represented by small diagonals attaching to the various diagonals that attach directly to the main horizontal line. This kind of model is useful in visually assessing a number of conditions or events that may have a bearing on a production outcome. Fishbone diagrams are just one of several types of cause and effect diagrams that planners can use to minimize problems in a task. The same kinds of professionals who use fishbone diagrams may use histograms, pareto charts, scatter diagrams, control graphs, check sheets, or any number of other planning and troubleshooting tools. In more complex systems involving money or other variables, advanced planning might utilize tools that measure or quantify a variable condition in more abstract ways. Computers have made more kinds of projections in decision-making possible for human planners, and in the modern world of planning, fishbone diagrams represent a more concrete or basic planning tool.

Training Manual on Quality Assessment of Food Products

ADVANCEMENTS IN FOOD INSPECTION TOOLS


G. Sujatha1, D. Baskaran2
2

Assistant Professor, College of Food and Dairy Technology, Koduvalli, Chennai 600 052 Professor and Head, Department of Food Engineering, College of Food and Dairy Technology, Koduvalli, Chennai 600 052

The modern food inspector must think of himself/herself as a reviewer of the food safety control measures and a contributor to their improvement. Control measures must individually evolve continuously in response to technological advances and to the establishments own experience, and as part of what should be an equally evolving national food control system. Such improvements can also be very advantageous to the processor from a marketing standpoint. Product safety and quality are characteristics that can be exploited to gain advantage in the marketplace. The food inspector is in a unique position to convey these messages to food producers and processors. Creating awareness about food safety and quality among food producers and processors is as important an element of food inspection as verifying compliance with regulations. Improvements to a quality and safety management system are almost always possible and attainable if the processor is willing to progress and the inspector is able to assist. A generalized trend in modern food processing safety and quality assurance systems is the concept of statistical process control (SPC), which is based on continuous improvement. Although this topic has dealt with SPC only marginally, when discussing critical limits, disseminating the concept of continuous improvement of the quality and safety management system and actively contributing to such improvement must be integral parts of food inspections.Food inspectors monitor food distributors, processors and manufacturers for safety and sanitation violations that could lead to food being contamination with adulterants or bacteria. They may inspect live animals and carcasses at a slaughterhouse or examine food imports at a port for mislabeling or other food safety issues. Inspectors report violations to the appropriate regulatory agency and are responsible for ensuring that foods are suitable for human consumption. Basic inspection tools 1. Pen and pencil 2. Writing tablet 3. Notebook 4. Inspection forms 5. Watch 6. Gloves 7. Aprons 8. Microbiological Sample Kit for Total Plate Count (by 3M) (optional) 9. Flashlight 10. UV light (optional)

Training Manual on Quality Assessment of Food Products

11. Thermometer 12. Copies of Laws and Regulations 13. Hair nets Nature of inspection tools 1. 2. 3. 4. 5. 6. 7. 8. 9. Portable, preferably small and lightweight, non-reactive, rugged and safe to use. Disposable or easily cleaned and decontaminated or easily protected from contamination. Relatively inexpensive. If powered tools, should run on standard batteries. Easy to replace any battery readily available from most convenience stores. Expendable materials used with any instrument should be non-proprietary; Simple and easy to operate with one hand because our other hand is generally holding a notebook, pen and flashlight. Accurate and easy to read, even in poor lighting conditions. Easy to calibrate or validate in the field. Capable of maintaining accuracy during hard use.

10. Not subjected to interference or damage by adverse environmental conditions or during transportation 11. Direct read or requiring only minimal interpretation of results. 12. Conforms to standards or standard protocols whenever possible or practical. 13. If any part of the instrument comes into contact with food, it should be non-toxic instruments to be versatile. ADVANCEMENTS IN INSPECTION TOOLS The Food Code also defines potentially hazardous foods in terms of water activity (AW) and pH, and the interaction of the two under certain conditions. Therefore, any comprehensive food safety evaluation of retail food establishments must include the monitoring of these two parameters. Water Activity. There are a few very good portable water activity monitors offered in the marketplace. They are similar to the pen-type hygrometer and not really easy to operate. About five years ago, Decagon Devices, Inc. introduced the easy-to-use and compact Pawkit. The Pawkit is a small, lightweight, albeit rather pricey, field kit for measuring water activity in foods. Pawkit for measuring ambient relative humidity, if conditions call for it. Measuring water activity with the Pawkit is relatively simpleCalibration is also easy to check and adjust whenever necessary. The kit contains everything needed for field work including the instrument, sample cups and verification standards.

10

Training Manual on Quality Assessment of Food Products

Measuring pH. For some inexplicable reason, The pH pens do well back in the lab but whether it is the jarring or temperature extremes from transporting them to the job site, it seems that food inspectors always have to rely on some other method for pH screening. Refractometers There is always another way to characterize potentially hazardous foods from those that are not potentially hazardous: refractometry. Consider purchasing inexpensive handheld sugar/Brix and salinity refractometers to measure syrups and brines. Refractometers are available through most scientific suppliers. The Food Code guidelines necessitate the use of several types of food safety inspection instruments, including light meters, single-use paper thermometers, and sanitizer indicator papers. Light Meter The food inspectors are partial to the General Electric (GE) Type 217 light meter available through most scientific catalogs. It is the ideal portable instrument: smaller than the typical size of a digital unit, rugged, versatile and lightweight and it uses the light it measures as its energy sourcetherefore, no batteries. The only drawback is that it cannot measure illumination below 10 candles. Single-Use Paper Thermometer It is a thermocouple thermometer with an Atkins 50415 dishwasher probe. However, for routine inspections and day-today quality assurance the paper thermometer are found to be convenient and quite accurate. They have the following advantages like the self-adhering label works on any clean porcelain or metal surface, Thermolabel measures the temperature on a heat-sink (which implies a dwell time), the label is accurate to within 1% of the calibrated temperature and the label is removable and can be repasted on the inspection report and serve as a permanent record Sanitizer Indicator Papers The reaction on most chlorine indicating papers is a change in the intensity of blue color. The food inspectors use Code 4250-BJ, acid-free LaMotte Chlorine Test Papers, whose end-point color is probably the easiest to interpret. Quaternary ammonium chloride sanitizers, however, are measured with pH. The pHydrion QT-40 test papers, manufactured by Micro Essential Laboratory, relies on color change. The comparator with each roll pack is already given in parts per million (ppm). Micro Essential Laboratory has a wide variety of sanitizers. Flashlights It uses the basic AA-cell type halogen flashlight featuring one-handed operation. The latest constant companion is the Streamlight 4AA ProPolymer LED flashlight. This flashlight uses four AA batteries and features seven LED bulbs that produce an extremely intense white light.
Training Manual on Quality Assessment of Food Products 11

While this flashlight cannot be adjusted to produce a spot, its light provides startling visual contrast, thereby making it easier to spot insect and rodent damage, water leaks and chronic wetness, and general soiling. The flashlight is ruggedly built and features a protected on/off switch. The battery life far exceeds that of the halogen lights. LED flashlight 80 lumen directed light beam of the Infinition shows everything and is indeed the best tool for any inspection UV Light ultraviolet (UV) light to a food safety audit because of its size and weight. However, in the past year the Emissive Energy Corp. introduced theInova X5 UV flashlight. The Inova X5 is a small (4.75"), hand-held LED powerhouse that uses five super-bright UVLEDs to produce abroad smooth pattern of light. For the first time, we now have a flashlight bright enough to detect rodent urine and mold. It is quite handy to qualify the level of cleanliness in restrooms. The Inova X5 uses two 3V lithium batteries and comes with an open-top nylon belt holster. Ground Fault Interrupter Electrical Safety to small instruments to ensure our safety (and that of the employees), and to detect most electrical problems. The A/C Sensor, which is slightly larger than a pen, simply indicates the presence of electrical current when held close to a live source or piece of equipment. A ground fault circuit interrupter/receptacle tester is also needed to check the wiring configuration of outlets, as well as the Ground Fault Interrupter (GFI). Both are available in most hardware stores. Ventilation. to characterize ventilation, particularly direction and flow, the Flowchecker. A small squeeze bottle that contains amorphous silicon dioxide powder available from Lab Safety Supply. For something a bit less expensive, try a zinc stearate powder in a small, empty nasal spray bottle is complemented with an inexpensive and compact Dwyer 460 Air Meter. Other miscellaneous includes 8 tape Measure, a pen-sized door pressure gauge and a 1:20/1:12 ramp-slope bubble measuring device, pressure gauge and ramp-slope bubble measuring device are manufactured by HMC International of Littleton, CO are also used in addition to all of the above, the basic food safety field kit also contains the following: 1. 2. 3. 4. 5. 6. 7. 8.
12

Wooden-stick cotton swabs to show where the dirt really is. A collapsible inspection mirror (Sears Craftsman) to see where the dirt really is. A small awl or ice pick for a thousand and one uses. Alcohol wipes. Self-sealing, quart-sized plastic bags. Vinyl disposable exam gloves (sensitive to latex allergies). A small blade and Phillips screwdriver and tweezers. A Mellon tester pocket knife and/or an electricians knife.
Training Manual on Quality Assessment of Food Products

SAMPLING OF FOOD PRODUCTS


Dr. P. Selvan
Assistant Professor, College of Food and Dairy Technology

INTRODUCTION To control food quality and acceptance within satisfactory limits, it is important to monitor the vital characteristics of raw materials, ingredients, and processed foods. This could be done by evaluating all foods or ingredients from a particular lot, which is feasible if the analytical technique is rapid and non-destructive. However, it is usually more practical to select a portion of the total product volume and assume the quality of the selected portion is typical of the whole lot. Obtaining a portion, or sample, that is representative of the whole is referred to as sampling, and the total quantity from which a sample is obtained is called the population. Adequate sampling technique helps to ensure that sample quality measurements are an accurate and precise estimate of the quantity of the population. By sampling only a fraction of the population, a quality estimate can be obtained more quickly and with less expense and personnel time than if the total population were measured. The sample is only an estimate of the value of the population, but with proper sampling technique, it can be a very accurate estimate. SAMPLE COLLECTION It is important to clearly define the population that is to be sampled. The population may vary in size from a production lot, a days production, to the contents of a warehouse. Extrapolating information obtained from a sample of a production lot to the population of the lot can be done accurately, but conclusions cannot be drawn from data describing larger populations, such as the whole warehouse. Populations may be finite, such as the size of a lot, or infinite, such as in the number of temperature observations made of a lot over time. For finite populations, sampling provides an estimate of lot quality. In contrast, sampling from infinite populations provides information about a process. Regardless of the population type, that is, finite or infinite, the data obtained from sampling are compared to a range of acceptable values to ensure the population sampled is within specifications. i. Homogeneous Versus Heterogeneous Populations The ideal population would be uniform throughout and identical at all locations. Such a population would be homogeneous. Sampling from such a population is simple, as a sample can be taken from any location and the analytical data obtained will be representative of the whole. However, this occurs rarely, as even in an apparently uniform product, such as sugar syrup, suspended particles and sediments in a few places may render the population heterogeneous. In fact, most populations that are sampled are heterogeneous. Therefore, the location within a population where a sample is taken will affect the subsequent data obtained. However, sampling plans and sample preparation can make the sample representative of the population or take heterogeneity into account in some other way. ii. Manual Versus Continuous Sampling To obtain a manual sample the person taking the sample must attempt to take a random sample to avoid human bias in the sampling method. Thus, the sample must be taken from a number of locations within the population to ensure it is representative of the whole population. For liquids in
Training Manual on Quality Assessment of Food Products 13

small containers, this can be done by shaking prior to sampling. When sampling from a large volume of liquid, such as that stored in silos, aeration ensures a homogeneous unit. Liquids may be sampled by pipetting, pumping, or dipping. However, when sampling grain from a rail car, mixing is impossible and samples are obtained by probing from several points at random within the rail car. Such manual sampling of granular or powdered material is usually achieved with triers or probes that are inserted into the population at several locations. Errors may occur in sampling, as rounded particles may flow into the sampling compartments more easily than angular ones. Similarly, hygroscopic materials flow more readily into the sampling devices than does non hygroscopic material. Horizontal core samples have been found to contain a larger proportion of smaller-sized particles than vertical ones. Continuous sampling is performed mechanically. iii. Importance of Sample Collection The reliability of analytical data thus obtained depends on several factors, sampling being the major factor. Current analytical methods require only few grams of food sample to analyze. Thus, it is necessary that a sample be as representative of the population as possible. There are three basic activities involved in analysis of food products:

Collection of representative sample. Sample preparation. Analysis using appropriate methods and instruments.

These activities, although independent in nature, yet can have decisive influence on each other. Furthermore, each of these activities have their own potential sources of variations that contribute to the uncertainty level associated with any analytical result. Thus, care must be taken to identify the sources of variation and minimize or avoid them while accomplishing any activity. On the part of the laboratories, it is therefore necessary to develop a plan for the proper performance of each activity, and then establish quality standards and written procedures in compliance with the standards. Many times, the activity of sampling falls outside the purview of a laboratorys mandate or control. This is especially true in commercial testing laboratories where the first contact is the arrival of samples. To improve the overall quality of the analytical process, a laboratory must do all it can to receive appropriate, applicable, defensible samples. The development of appropriate plans will depend upon an understanding of the problems involved in each activity, and then the application of reasonable judgments in seeking solutions. It should be noted that sampling terminology and procedures used may vary between companies and between specific applications. However, the principles described in this Unit are intended to provide a basis for understanding, developing, and evaluating sampling plans and sample handling procedures for specific applications encountered. A sample should represent a population as adequately as possible. To ensure proper sampling, the analysts need to be consulted time to time concerning proper sample size, suitable containers for sampling or the use of appropriate preservatives to prevent any spoilage or transformation in a sample before analysis. One common cause of lack of precision or lab-to-lab variation in analytical results for a particular population can be traced back to erroneous sampling. For example, in case of grapes, a laboratory sample size of meager 3 kg berries represents the whole population of > 10000 kg in 1 hectare vineyard area. Thus, if the sample collected is not representative, then there will be sample-to-sample variation in results. When significant difference in results occurs among laboratories which have supposedly analyzed the same sample, a serious conflict may arise questioning the competence and credibility of the laboratories.
14 Training Manual on Quality Assessment of Food Products

Many of these situations can be avoided if samples are collected according to a rational plan that gives some assurance that the sample delivered to the laboratory represents the composition of the parent lot. There are at least two ways to measure a given lot of goods: one, that we often assume to be the proper way, is to find its true value, by which we mean its average value. The other way, often discovered accidentally as a result of poor sampling, is to measure its variability. So called proper sampling of drug dosage forms, for example, may involve compositing 20 tablets, by which the majority of the tablets could be used to dilute and conceal the fact that several of them are severely sub- or superpotent. Similarly, two lots of grain may have been purposely, but ineffectively, mixed in an attempt to reduce the average level of a contaminant. Sampling that led to the laboratory finding inconsistent results would reveal the attempt to dilute an illegal product. iv. Errors in Analytical Results due to Improper Sampling Few studies have been conducted on the distribution of error among the three activities: sampling, sample preparation, and analysis. In one such study, which involved analysis of 20 nanogram/gram concentration of aflatoxin in a lot of peanuts, the error contributed by the sampling step was as high as 67% of the total variance, in comparison to 20% and 13% errors contributed by the analyst and the analytical procedure, respectively. In a field study conducted at the National Research Centre for Grapes, Pune, the pesticide residues in grape samples analyzed in 15 individual grape bunches collected out of 1 acre area showed above 50% sampling-induced variations. The results of such experimentations are not unusual and it illustrates the proportion of error that can be attributed to sampling. For peanuts, the distribution of aflatoxin can vary widely, with a few peanuts accounting for most of the contamination. Similarly, in case of the field sampling of grapes, the pesticide residues might have deposited in variable concentrations in different grape bunches and thus when they were analyzed separately, showed variable results. The important point in these examples is to show that sampling error can play a very significant part in the overall error in the analytical system. v. Risks Associated with Sampling There are two types of risks associated with sampling. Both should be considered when developing a sampling plan. The consumer risk describes the probability of accepting a poor quality population. This should happen rarely (<5% of the lots) but the actual acceptable probability of a consumer risk depends on the consequences associated with accepting an unacceptable lot. These may vary from major health hazards and subsequent fatalities to a lot being of slightly lower quality than standard lots. Obviously, the former demands a low or no probability of occurring whereas the latter would be allowed to occur more frequently. The second risk i.e., vendor risk is the probability of rejecting an acceptable product. As with consumer risk, the consequences of an error determine the acceptable probability of the risk. An acceptable probability of vendor risk is usually 5-10%. SAMPLING STANDARDS Data obtained from an analytical technique are the result of a stepwise procedure from sampling, to sample preparation, laboratory analysis, data processing, and data interpretation. There is a potential for error at each step and the uncertainty, or reliability, of the final result depends on the cumulative errors at each stage. Variance is an estimate of the uncertainty. The total variance of the whole testing procedure is equal to the sum of the variances associated with each step of the sampling procedure and represents the precision of the process. Precision is a measure of the reproducibility of the data. In
Training Manual on Quality Assessment of Food Products 15

contrast, accuracy is a measure of how close the data are to the true value. The most efficient way to improve accuracy is to improve the reliability of the step with the greatest variance. Frequently, this is the initial sampling step. The reliability of sampling is dependent more on the sample size than on the population size. The larger the sample size, the more reliable the sampling. However, sample size is limited by time, cost, sampling methods, and the logistics of sample handling, analysis, and data processing. It should be noted that sampling terminology and procedures used may vary between companies and between specific applications. Several standards and recommendations provide the ways and means to sample a particular lot. THE SAMPLING PLAN Understanding a Sample Plan Sampling is generally done for a specific purpose and the purpose may indeed suggest or dictate the nature of any sampling plan. The International Union of Pure and Applied Chemistry (IUPAC) defines a sampling plan as a predetermined procedure for the selection, withdrawal, preservation, transportation, and preparation of the portions to be removed from a lot as samples. A sampling plan should be a well-organized document that establishes the required procedures for accomplishing the programs objectives. It should address the issues of who, what, where, why, and how. The primary aim of sampling is to obtain a sample, subject to constraints on size, that will satisfy the sampling plan specifications. A sampling plan should be selected on the basis of the sampling objective, the study population, the statistical unit, the sample selection criteria, and the analysis procedures. The two primary objectives of sampling are often to estimate the average value of a characteristic and determine if the average value meets the specifications defined in the sampling plan. The presence of a well designed plan is important because it provides a consistent model to guide people performing the sampling activity, and it serves as a reminder of the important elements in this part of the overall sample analysis program. Statistical Approaches In many sampling programs, statistical approaches are not given the requisite attention. Percentage sampling systems that specify a fixed percentage of a lot, say 5 or 10%, do not provide the quality protection that is often assumed. Statistical sampling theory furnishes the means to analyze the relationship between a lot of goods and the samples that are drawn from it. It can be used to estimate population measure, or parameters, such as variance and correlation, from knowledge of corresponding samples quantities. The importance of sampling is recognized in ISO 17025, which requires that test reports make reference to the sampling procedure used by the laboratory or the submitting body. SAMPLING TECHNIQUES/METHODS There are several sampling methods/techniques in common use. These are probability sampling, non-probability sampling, bulk sampling, and acceptance sampling. These are described in brief below: Probability Sampling Probability sampling is used when a representative sample is desired, and uses principles of statistical sampling and probability i.e. elimination of human bias. It is a random selection approach that tends to give each unit an equal chance of being selected.
16 Training Manual on Quality Assessment of Food Products

Simple random sampling requires that the number of units in the population be known and each unit is assigned a number. A specific quantity of random numbers between one and total number of population units is selected. Sample size is determined by lot size and potential impact of a consumer or vendor error. Units corresponding to the random numbers are then analyzed as an estimate of the population. Systematic sampling is used when a complete list of sample units is not available, but when samples are distributed evenly over time or space, such as on a production line. The first sample is selected at random and then every nth unit after that. Stratified sampling involves dividing the population into overlapping subgroups so that each subgroup is as homogenous as possible. Group means, therefore, differ from each other as much as possible. Random samples are then taken from each subgroup. The procedure provides a representative sample because no part of the population is excluded and it is less expensive than simple random sampling. Cluster sampling entails dividing the population into clusters or subgroups so that clusters characteristics are as identical as possible, that is, the means are very similar to each other. Any heterogeneity occurs within each cluster. Clusters should be small and having a similar number of units in each cluster. The clusters are sampled randomly and may be either totally inspected or subsampled for analysis. This sampling method is more efficient and less expensive than simple random sampling, if populations can be divided into homogenous groups. Composite sampling is used to obtain samples from bagged products such as flour, seeds, and larger items in bulk. Two or more samples are combined to obtain one sample for analysis that reduces differences between samples. For example, FDA composite 12 and at least six subsamples, respectively, for the sample to be analyzed for compliance with nutrition labeling regulations. Non-probability Sampling Non-probability sampling is used when it is not possible to collect a representative sample, or a representative sample is not desired. For example, in case of adulteration such as rodent contamination, the objective of the sampling plan may be to highlight the adulteration rather than collect a representative sample of the population. The sample collector uses judgment rather than statistical considerations in the selection of the sample. The unusual or unexpected characteristics in a population could be selected to be identified. This type of sampling is done in many ways, but in each case the probability of including any specific portion of the population is not equal because the investigator selects the samples without estimating sampling error. Judgement sampling is solely at the discretion of the sampler and therefore is highly dependent on the person taking the sample. This method is used when it is the only practical way of obtaining the sample. This method may present a better estimate of the population than random sampling if sampling is done by an experienced individual and limitations of extrapolations from the results are understood. Convenience sampling is performed when ease of sampling is the key factor. The first pallet in a lot or the sample that is most accessible is selected. This type of sampling will not be representative of the population, and therefore is not recommended.

Training Manual on Quality Assessment of Food Products

17

Restricted sampling may be unavoidable when the entire population is not accessible. For example, if sample is to be taken from a loaded truck, but the sample is not a representative of the entire population. Quota sampling is the division of a lot into groups representing various categories, and samples are then taken from each group. This method is less expensive than random sampling but also is less reliable. Types of Sampling A) Bulk sampling Bulk sampling involves the selection of a sample from a lot of material that does not consist of discrete, identifiable or constant units. Sampling may be performed in static or dynamic situations. Bulk sampling poses special problems requiring certain decisions to be made: the number of increments to be taken, the size of the increments, from where in the pile or stream they should be drawn, the sampling device to be used, and how to reduce the increments taken to a reasonable size of sample for delivery to the laboratory. B) Acceptance sampling Acceptance sampling differs from the previous types and involves the application of a predetermined plan to decide whether a lot of goods meet defined criteria for acceptance. The risks of accepting bad or rejecting good lots are stated in conjunction with one or more parameters, for example, quality indices of the plan. Statistical plans can be designed to regulate the probabilities of rejecting good lots or accepting bad lots. There are two broad categories of acceptance sampling: sampling by attributes and sampling by variables. Sampling by attributes In sampling by attributes, the unit of product is classified as defective or nondefective, or the number of defects in a unit of product is counted with respect to a given requirement. Or, the sampling is performed to decide on the acceptability of a population based on whether the sample possesses a certain characteristic, for example, Clostridium botulinum contamination in canned goods. An example of net weight determination may serve to explain the differences between the two categories. In attribute sampling, each unit that weighs 1 pound or more is accepted, and each unit that weighs less than 1 pound is rejected. If the number of rejects exceeds a predetermined number, the lot is rejected. If the number of rejects is less than the predetermined number, the lot is accepted. Sampling by variables In variable sampling, sampling is performed to estimate quantitatively the amount of a substance (e.g., salt) or a characteristic (e.g., color) on a continuous scale. The estimate obtained from the sample is compared with an acceptable value (i.e., previously determined) and the deviation measured. This type of sampling usually produces data that have a normal distribution such as in the per cent fill of a container and total solids of a food sample. In general, variable sampling requires smaller sample size than attribute sampling and each characteristic should be sampled for separately when possible.

18

Training Manual on Quality Assessment of Food Products

Operating Characteristic (OC) Curves Operating Characteristic (OC) curves are used extensively in acceptance sampling. The OC curve shows the relationship between the quality and the per cent of lots expected to be acceptable for the quality characteristic inspected. In other words, the OC curve is a graph of lot defectives against the probability that the sampling plan will accept the lot. The Operating Characteristic (OC) curve shows the probability of acceptance, Pa, for any level of lot quality. On the horizontal axis is the quality characteristic. This OC curve enables you to evaluate the probability of acceptance for any true lot quality level-on a what-if basis. This way, you can design sampling plans that perform the way you want. Requirements of Good Sampling Methods Samples are useful for their intended purpose when they are taken in a manner consistent with generally recognized good sampling techniques and good sampling practices. This requires the following:

Inspection of the lot before sampling. Use of suitable sampling devices for the particular commodity and type of sample desired. Use of suitable containers to hold the sample. Maintenance of the integrity of the sample and associated records. Use of adequate precautions in preserving, packing and delivery of the sample to the lab in a timely manner. Provision of appropriate storage conditions for the sample both prior to and following analysis.

All of these factors, along with others such as cost versus benefits analysis, and a review of program objectives and regularity requirements, are to be assessed and brought together in a sampling plan that serves as a guide to management, as well as to operating personnel as a firm plan to achieve quality in sampling. Cost of Sampling The attention of users is drawn upon relation between the efficiency and size of sample. For a given Acceptable Quality Level (AQL), the smaller the sample size, the smaller the cost of sampling, but the worse the efficiency, that is the risk to wrongly accepting a lot increases and worsens the damage in trade. Problems in Sampling Analytical data never are more reliable than the sampling technique. Sampling bias, due to nonstatistically viable convenience, may compromise reliability. Errors also may be introduced by not understanding the population distribution and subsequent selection of an inappropriate sampling plan. Unreliable data also can be obtained by non-statistical factors such as poor sample storage resulting in sample degradation. Samples should be stored in a container that protects the sample from moisture and other environmental factors that may affect the sample (e.g., heat, light, air). To protect against changes in moisture content, samples should be stored in an airtight container. Light sensitive samples
Training Manual on Quality Assessment of Food Products 19

should be stored in containers made of opaque glass, or the container wrapped in aluminum foil. Oxygen sensitive samples should be stored under nitrogen or an inert gas. Refrigeration or freezing may be necessary to protect chemically unstable samples. However, freezing should be avoided when storing unstable emulsions. Preservatives (e.g., mercuric chloride, potassium dichromate, and chloroform) can be used to stabilize certain food substances during storage. Mislabeling of samples causes mistaken sample identification. Samples should be clearly identified by markings on the sample container in a manner such that markings will not be removed or damaged during storage and transport. For example, plastic bags that are to be stored in ice water should be marked with water-insoluble ink. If the sample is an official or legal sample the container must be sealed to protect against tampering and the seal mark easily identified. Official samples also must include the date of sampling with the name and signature of the sampling agent. The chain of custody of such samples must be identified clearly. THREE CLASS SAMPLING PLAN Another type of sampling used frequently by regulatory agencies to determine acceptance or rejection of a lot (often defined as the quality of product produced under essentially the same conditions but representing no more than one days production) is the three-class sampling plan. This approach is often used when assessing microbiological contamination of foods. In this case, n is the number of samples, usually selected at random from the lot, the numerical value m represents acceptable concentrations, the numerical value M represents un-acceptable concentrations, and c is the maximum allowable number of marginally acceptable sample units such that if this number is exceeded, the lot is considered as un-acceptable. While m separates sample units of acceptable quality from those of marginally acceptable quality, M separates sample units of marginally acceptable quality from those of defective quality. For enforcement purposes, the sampling technique used should be the same as the sampling technique used to set the standard. For example, minimum reportable limits for particles are based on composite samples and not on individual lots. PREPARATION OF SAMPLING PLANS The development of quality sampling plans is a science in itself and has been given consideration by a number of organizations. One plan format that deserves serious consideration, developed by the International Organization for Standardization, is shown with comments in ISO/TC 34, ISO/DIS 7002.2, Agricultural food products- Layout for a standard method of sampling from a lot (1988). It can serve as a starting point or check list for developing a sampling plan for most commodities. The title and headings from sections in the monograph are as below: Model Sampling Plan Agricultural food products- Layout for a standard method of sampling from a lot. 1) Title (short but appropriate for index identification) 2) Introduction (describing the purpose of the plan) 3) Scope (describing the breadth of coverage of the plan) 4) Field of application (products to be covered; where sampling will be done)
20 Training Manual on Quality Assessment of Food Products

5) References (documents, the validity of the plan with reference to other requirements) 6) Definitions (specific terms associate with a particular matrix) 7) Principle (statistical basis of the method of sampling) 8) Administrative arrangements a) Sampling personnel b) Representation of parties concerned c) Health, safety and security precautions d) Preparation of the sampling report 9) Identification and inspection of the lot prior to sampling (important in survey sampling for identification, condition of the lot and selection of method of sampling). 10) Sampling equipment and ambient conditions (proper tools such as use of sterile equipment for aseptic sampling). 11) Sample containers and packing (essential to prevent contamination and damage during shipment or storage). 12) Sampling procedures (as dictated by the plan objectives). a) Sampling size b) Taking the sample. c) Preparation of bulk samples and reduced samples d) Selection of samples of pre-packaged products. 13) Packing, sealing and marking of samples and sample containers (identification of units and to establish chain-of-custody). a) Filling and sealing sample containers. b) Labeling or marking (including signature of sampling personnel). c) Packing samples for storage or transportation. 14) Precautions during storage and transportation of samples. 15) Sampling report a) Administrative details. b) Details of unit packs or enclosure containing the lot. c) Material samples. d) Marking and sealing of samples. 16) Annexure (supplemental information, if necessary).

Training Manual on Quality Assessment of Food Products

21

SUB SAMPLING FOR ANALYSIS AND TAKING THE TEST PORTION If the test portion analyzed does not represent the sample or the lot from which it was taken, in that case, even the best analysis could give misleading information. Distortions introduced at this point will carry through the path of analysis and adversely affect the final results and the conclusions drawn from them. There are generally two choices in analytical sub sampling:

Preparation of a composite laboratory sample (if multiple units are submitted for analysis). Examination of individual units.

Composite Lab Sample Preparation A composite lab sample is one in which the individual units or representative portions of units are mixed to form a uniform mixture. Portions are then taken from the composite for analysis. Compositing saves analytical time and in some types of contract testing it may be the procedure specified. If the results indicate that there may be a problem, it will likely be necessary to go back and analyze individual samples. Compositing is not the procedure of choice when there is a chance that an individual unit that constitutes a public health or safety threats will not be detected (there are some exceptions) or where a unit at or outside of tolerance level will not be detected because of matrix dilutions. Multiple unit lab sampling is indicated when the possible range of values among individual units is considered significant or it is desirable to establish the variability of the lot. Opinions of Experts You den and Steiner (Statistical Manual of the AOAC, AOAC International, Arlington, VA, p 41) observed that, Many materials are notoriously difficult to sample. Often the variability among samples is the controlling factor in the confidence placed in the analytical result. They note further that A mistake sometimes made is to composite several samples and then to run repeat determinations on this composite sample. The analyst may be happy with several results that are in close agreement because only the analytical error is involved in the results. And some may put their faith in the result admittedly, if the individual samples were of the same weight and properly mixed, the same average will result whether the samples are analyzed individually or repeats are made on the composition. Using the composite sample effectively conceals the between-sample variation. It should be mandatory to run the samples individually, for only by doing so will anybody be in a position to make any statistical statements about the results, no matter how good the analytical procedure. Somewhat similar view of sub sampling for analysis is expressed in an article published in Chemical and Engineering news by an ad hoc sub committee of The American Chemical society for Dealing with the Scientific Aspects of Regularity Measurements. This report observes that the number of samples to be analyzed in a given situation usually is limited by the resources available for collection of samples or for their analysis. However, the reliability of the result generally increases with the square root of the number of samples analyzed. For this reason, analysis of multiple samples are preferred over single samples since, single samples give no information on the homogeneity of the lot that was sampled. In addition, for single samples, the sampling error is also confounded with theanalytical error. As a result, if the total number of determinations must be fixed, multiple independent single samples are preferred over replicate aliquots per a single random sample. In any case, the sampling decisions should be a priori decision and should be based on the question at issue.

22

Training Manual on Quality Assessment of Food Products

In addition to the number of sub samples taken for analysis, it is essential that each be prepared in a way that achieves homogeneity and is handled in a manner that prevents alteration from the original composition. Obviously, failure to prepare a homogeneous sub sample at this point will affect the results of the analysis regardless of the method used. SAMPLE PREPARATION FOR ANALYSIS Every type of material that is to be prepared for analysis presents its own practical difficulties. The requirements for suitable sample preparation are dictated by the consistency and the chemical characteristics of the analyte and the matrix, and by the distribution of the analyte in the sample. Even seemingly homogeneous materials such as liquids may be subject to sedimentation or stratification. Thus, vigilance and care are the watch words to ensure homogeneity. Precautions to be followed while Preparing a Sample for Analysis Mixing: Single phase liquids can generally be mixed, stirred, shaken or blended. Dry particulate materials can be reduced in the volume by coning and quartering, by rolling and quartering, or by the use of a splitter, such as a refill. A variety of implements and machines are available for sample disintegration, such as mills, grinders and cutters. Care in their use is necessary to prevent loss of dust or change in composition through partial separation of components. Screening can be used to improve the efficiency of particle size reduction, followed by mixing to attain homogeneity. Sampling errors can occur even in well mixed particulate mixtures especially in trace analysis if the particles differ appreciably in size or physical properties. Cleanliness of equipment used in process Every piece of equipment used in the preparation of a sample must be examined critically to ensure their cleanliness, so that they do not contaminate or decompose or cause any physical loss of the sample while processing. Grinders were mentioned above as contributing to the loss of finer particles as dust. They have been known to segregate materials with in the mix by size as well, with the finer material, collecting beneath the blade e.g., Metal screens can pass fine particles, but retain powder that adheres to the screen materials. Glass containers and laboratory apparatus can adsorb certain materials and may require surface treatment. Plastic containers can retain contaminants, such as animal hairs, while the rest of the sample is transferred with apparent ease. In the other words, validation of a method of analysis, includes, most certainly validation of the method of sample preparation and storage. Changes in physical characteristics Loss or gain of moisture during processing can be a problem. Loss can be minimized by keeping samples covered with plastic or aluminum foil. A cold product can be protected from gaining moisture by allowing the sample to come to room temperature before preparation begins. High fat samples such as nuts may be difficult to grind without clogging up the grinder; one technique that is used is to freeze the samples prior to grinding. Changes in chemical characteristics When volatile organic constituents are present in any sample, processing may be difficult and needs special care, e.g. maintaining chilled condition to prevent any loss of volatile constituents. Similarly,
Training Manual on Quality Assessment of Food Products 23

in case of photo-sensitive chemicals (e.g. natural product pesticides), it is required to process a sample under darkness to prevent degradation on exposure to light. Portions for sampling As a general guide, food samples are analyzed in the form they are commonly consumed. Inedible portions, such as stones (e.g. for mango), nutshells, or fish bones are removed and discarded prior to analysis, and suitable note made of how the sample was prepared. The technique used for setting the standard should be used to ensure comparability. Sampling for Trace metals Trace metals analysis can present significant problems, For example, the trace metals can be distributed unequally between liquid and solid phases in pickles, canned vegetables and canned fruits. Obviously, such irregular distribution of metals can pose problems for the analyst in establishing the level of metal residues in the product, as well as for those concerned with setting tolerances. Thus, it becomes necessary to analyze both the solid and liquid phases. DIFFICULTIES IN SAMPLING As mentioned earlier, one of the most difficult problem in sampling from a lot, and in subsequent lab subsamples, is trying to obtain a representative sample for the analysis of aflatoxins in raw agricultural commodities. Aflatoxin contamination exhibits a highly erratic distribution, with a reduction in heterogeneity as the food or feed is reduced in particle size. After it was recognized that there was a high rate of variability and within same samples from the same lot, there was a moment towards the collection of larger and larger samples. Sample sizes started, for peanuts with 1 kg, and the size increased as more reliable results were required by food procedures (increasing sample size reduces the number of good lots that are likely to be rejected and the number of bad lots accepted). Example for Effect of Sampling on Analytical Result At the present time in the United States, the sample taken from a lot of shelled peanuts of 144 pounds; three 48 pounds samples with portions taken at random from the lot. Examination in the lab is by sequential analysis with first 48 pounds sample ground in a subsampling mill and test portions examined in duplicate. If the average of the test portions is below the established tolerance (set by US Food and Drug Administration), the lot is passed. If the average is above the acceptance level, the lot is rejected. If the findings fall between the two figures the second 48 pound sample is comminuted and the analysis repeated. If a decision cannot be made to accept or reject the lot, the third 48 pounds sample is prepared, assayed, and the cumulative results considered. The foregoing example point out dramatically the need for attention to lot sampling, lab subsampling, and sample preparation for analysis. While this is a rather extreme case, it illustrates that sampling problems cannot be ignored or treated indifferently. In Canada, while the specified sample sizes are smaller, ranging from 12 to 20 kg. depending on the commodity and the lot size, and minimum number of sampling sites are also stipulated to address the erratic distribution of aflatoxin contamination.
24 Training Manual on Quality Assessment of Food Products

SAMPLE ACCOUNTABILITY Documentation A laboratory sample is generally the starting point for analytical work. The sample may be delivered by mail, courier, flight, or directly by the collector. It may arrive in any of various containers and conditions: frozen, packed in ice, or at room temperature. The package may be sealed or unsealed, and the sample itself may be spoiled or broken. The sample may or may not be accompanied by appropriate documentation to advise the laboratory regarding purpose, test parameters and the conditions of storage, etc. Once a sample is received, all the circumstances and conditions must be documented as they could have bearing upon the quality or the significance of the test results. It is important for appropriate quality analysis that sample arrives in proper condition with meaningful documents. Procedures for these must be established, continually reviewed, and enforced, to keep poor sample handling and delivery to a minimum level. To avoid any future legal complications, the laboratories are advised to protect themselves with the cautionary statement in the test report indicating that the results relate only to the sample that was tested. Chain of Custody Form In most organizations specific sampling procedures are written and the sample collectors are trained regarding their responsibilities. The first important activity is the documentation to ensure product traceability. The sample should be easily identifiable and placed under seal and packing. Shipping and delivery instructions are followed to effect delivery to the laboratory. The documentation consists of a chain-of-custody that accompanies the sample as it moves through the laboratory and subsequent administrative handling. This form is usually prepared in multiple copies for distribution to various units in the organization, may be supplemented with affidavits, dealers statements, bills or other relevant information that concerns the sample, its origin, the transfers from one custodian to the next and the samples significance or importance. Information such as sample number, product name and identification, reason for collection, description of the sample and of the method of collection, size of the lot from which the sample was taken, codes, shipment information, collection date, name of the collector, means of transportation, and whether or not sealed are supplied with the sample. If the sample is sealed, the seal includes the sample number, date the seal was affixed, and the collectors signature. The seal is attached to the package in such a way that it must be broken before the sample can be obtained. Sample Receipt and Handling The next step in the sample accountability system is receipt of the sample in the laboratory. A dependable record of sample handling is important so that the sample is accepted by a sample custodian who documents the action by completing a sample accountability record. This document should contain the sample number, the name of the product and date received, indicate who received it, describe the method of shipment or delivery, describe the packages received and their condition, and provide space for recording various storage locations before and after analyses. Deliveries of the sample or portions of the sample to the analyst, and its return, will also be recorded on this form. There will be a signed statement concerning the final disposition of the reserve sample. A two-part form can be used for this purpose; one copy remains with the sample custodian and the other moves with the sample through the laboratory and is used by a supervisor for sample management purposes. Some laboratories
Training Manual on Quality Assessment of Food Products 25

use a sample receiving log book for sample control. The information entered in the log book is essentially the same as that described for the two-part form. Monitoring of Samples The sample accountability in a laboratory can be monitored by a simple computer program; a unique label should be generated and affixed to the sample container, and all the pertinent sample information should be entered into the computer database. The information entered at login becomes part of the data base, which is then built up through the manual or automatic addition of sample handling information and analytical data. Worksheet pages or reports can be calculated and printed, and the data base itself latter queried and manipulated for various information and reporting purposes. Regardless of the recording system used, the analytical information generally reported includes a description of the sample, subsampling procedure sample preparation methods used, deviations from methods, validation and recovery experiments (if performed), standards used, source of reference materials, raw data, calculations and description of the reserve sample and how it was prepared for storage after the completion of the analysis. In addition, pertinent supporting documents such as chromatograms, spectra, and other charts are suitably identified with instruments identification, operating conditions, analyst name, sample number and date. If the reserve sample is sealed, the information placed on the seal is shown in the report. The sample is then returned to the sample custodian to be stored for whatever future action may be necessary, or until the sample is destroyed. RETENTION OF SAMPLES AND RECORDS After an analysis is complete and the results reported, the laboratory needs a written policy for guidance on the retention of the samples and the associated records. For samples and records that may be involved in litigation, the storage period can extend for years. For the majority of samples, fortunately, this is not usually the case. The objective should be to destroy samples as soon as it can be analyzed, with certainty that they will no longer be required for further testing or as evidence. The records may be disposed after they are no longer legally or administratively important. Identify the Properties of Retained Samples It is very important for the laboratory management to determine whether or not the materials being discarded are hazardous in nature. Although samples themselves may not be hazardous, acid digestions and organic solvent extractions certainly can be hazardous. Sample management includes the proper disposal of samples and laboratory preparations. Standard operating procedures for samples for sample disposal are essential. Retention Period Storage periods, obviously, must be determined by each facility depending on its obligations, but clear policy must be in place to prevent both the destruction of important items, and the accumulation of what is essentially junk. From a quality assurance point of view, the improper destruction of active samples or records is low quality performance in violation of policy, and the Quality Assurance (QA) program must provide a means to detect such actions in an effort to prevent their recurrence.

26

Training Manual on Quality Assessment of Food Products

CHAPTER 2

Training Manual on Quality Assessment of Food Products

27

28

Training Manual on Quality Assessment of Food Products

QUALITY CONTROL OF MILK AND MILK PRODUCTS


Dr.D.Ramasamy
Professor, College of and Dairy Technology, Chennai-52

1.1. DEFINITION OF MILK Milk may be defined as the whole, fresh, clean lacteal secretion obtained by the complete milking of one or more healthy milchy animone-sixth as sweet as sucrose. Lactose is responsible for the defect known as sandiness in ice-cream or condensed milk. Milk Proteins : The proteins in milk consists mainly of casein, lactaglobulin, lactalbumin, milk serum albumin,fat. 1.2. CHEMICAL COMPOSITION OF MILK

Water: Water constitutes the medium in which the other milk constituents are either dissolved or suspended. Most of it is free and only a very small portion is in the bound form, being firmly bounded by milk proteins, phospholipids etc. Total Solids: Total Solids constituents lipids (Fat) and solid not fat. Milk Fat (Lipids): The bulk of the fat in the milk exists in the form of small globules, which average approximately 2 to 5 microns in size. This is an oil-in-water type emulsion. The fat associated substances are phospholipids, cholesterol, carotene and fat soluble vitamins (A, D, E, and K). Milk Sugar or Lactose: This exists in milk only. It is in true solution in the milk serum. On crystallization from water, it forms hard gritty crystals. It is one-sixth as sweet as sucrose. Lactose is responsible for the defect known as sandiness in ice-cream or condensed milk. Milk Proteins : The proteins in milk consists mainly of casein, lactaglobulin, lactalbumin, milk serum albumin, immuno globulins etc. Casein forms more than 80% of the total proteins of the milk. Casein exists only in milk and is found in the form of calcium caseinate phosphate complex. Lactalbumin and lactaglobulin are known as Whey or serum proteins. They are also present in colloidal state and are easily coagulated by heat. Milk serum albumin is same as blood serum albumin of the blood. Non protein nitrogenous Compounds : E.g. Ammonia, amino acids, protease-peptones, urea, uric acid etc.
Training Manual on Quality Assessment of Food Products 29

Mineral Matter or Ash : The mineral matter or salts of milk although present in small quantities, exert considerable influence on the physico- chemical properties and nutritive value of milk. Other Constituents Pigments: Water soluble pigments are Riboflevin and xanthophyll. Riboflavinbesides being a vitamin, is a greenish yellow pigment which gives characteristic colour to whey. Earlier it is known as lactoflavin or lactochrome. Dissolved Gases : Milk contains gases like O2, Co2, N2 etc. Vitamins : Water soluble vitamins B complex and vitamin C Enzymes : These are biological catalysts. Milk contains Amylase, Lipase, Phosphatase, protease, peroxidase and catalase enzymes. 1.3. NUTRITIVE VALUE OF MILK Milk is an almost ideal food. It has high nutritive value. It supplies body building proteins, bone forming minerals and health giving vitamins and furnishes energy giving lactose and milk fat. All these properties make milk an important food for pregnant mother, growing children, adolescents, adults, invalids, convalescents and patients alike. Proteins: Milk proteins are complete proteins of high quality i.e. They contain all the essential amino acids in fairly large quantities. Fat: Milk fat (lipid) play a significant role in the nutritive value, flavour and physical properties of milk and milk products. Besides serving as rich source of energy, fat contains significant amounts of so called essential fatty acids (linoleic and arachidonic). Lactose: The principle function of lactose (carbohydrade) is to supply energy. However lactose also helps to establish a mildy acidic condition in the intestine (which checks the growth of proteolytic bacteria) and facilities assimilation. Minerals: Practically all the mineral elements found in milk are essential for nutrition. Milk is an excellent source of calcium and phosphorus, both of which together with vitamin D are essential for bone formation. Milk is rather low in Iron, Copper and Iodine. Vitamins: These are accessory food factors, which are essential for normal growth, health and reproduction of living organisms. Milk is a good source of vitamin A (provided the cow is fed with green feed and fodder), vitamin D (provided the cow is exposed to enough sun light) thiamine, riboflavine etc. However milk is deficient in Vitamin C. Energy: The energy giving milk constituents and their individual contributions are as follows Milk Fat Milk proteins Milk Sugar 9.3C / g 4.1C / g 4.1C / g

30

Training Manual on Quality Assessment of Food Products

The energy value of milk vary with its composition on average cow milk furnishes 75C / 100 g and buffalo milk 100C / 100 g of milk. 1.4. PHYSICOCHEMICAL PROPERTIES OF MILK COLOUR AND FLAVOUR The colours of milks are Buffalo Milk Cows Milk Skim Milk Whey Creamy White Yellowish creamy white Bluish Greenish yellow (This is due to pigment Riboflavin).

The intensity of yellow colour of cow milk depends on various factors such as breed, feeds, size of fat globules, fat percentage of milk. The greater intake of green feed, the deeper the colour of cow milk. The larger the fat globules and the higher the fat percentage, the greater the intensity of the yellow colour. Flavour The freshly drawn milk has certain cowy odour which passes off by the time reaches the consumer. With the development of lactic acid the flavour also changes tosour. This is due to lactic acid, butyric acid and diacetyl. pH AND ACIDITY The hydrogen ion concentration of milk is about 10-66 gms per litre that is in terms of pH value it is 6.6. Freshly drawn milk is amphoteric to litmus i.e. it turns red litmus to blue and blue litmus red. The pH of cow milk is 6.4 -6.6 and buffalo milk 6.7 6.8. Higher pH values in freshly drawn milk indicates mastitis. SPECIFIC GRAVITY OF MILK The density of a substance is its mass (weight per unit volume). Specific gravity is the ratio of density of the substance to the density of standard substance (water). The specific gravity of milk is usually expressed at 60oF (15.6oC). Milk is heavier than water. The average specific gravities are Cow Milk Buffalo Milk Skim Milk 1.028 to 1.030 1.030 to 1.032 1.035 1.037

2. QUALITY CONTROL TESTS FOR MILK When milk is received on the platform, it has to undergo a number of examinations and tests. These tests are carried out to determine the quality of incoming milk and it is on the basis of these tests
Training Manual on Quality Assessment of Food Products 31

whether a particular lot is to be rejected. The most common of these are determination of fat%, SNF, total solids and sediments etc. 2.1. Organoleptic Test The sensory evaluation of milk is of utmost importance to the market milk industry. The sale of fresh milk is a major activity of the Indian dairy industry. Since milk is consumed in the liquid state by all classes of people, it is judged daily be the consumers. All the five senses viz., sight, smell taste, touch and sound are used in judging and grading of milk. Objectives To accept/reject raw milk on the basis of sensory observations. Procedure Removal of lid of the can Smell the milk and lid in case of any doubt, taste it by putting a small quantity on the tongue and spit it out in a spittoon. Feel the coldness/warmth of milk from outside the can. In case of Doubt, temperature may be observed with the help of a thermometer. Observe for any abnormality in colour and extraneous matter in milk. Observations

Smell/odour Taste Colour Sediment Temperature

2.2. Correct Lactometer Reading (C.L.R.) The estimates the amount of solid-not-fat (SNF) present in the milk sample. For this purpose Lactometer is used. Prior to filling the metallic cylinder upto brims with milk sample the temperature of milk (29C) is noted. The lactometer is then inserted inside the cylinder containing milk, and the temperature of the milk is noted again. The scale of lactometer projecting above the milk gives the lactometer reading. If the temp. of the milk is 29C then the lactometer reading itself is taken as CLR and if the temperature is below or above 29C, then for each degree rise or fall of temperature 0.5C is added or deducted from the observed lactometer reading.

32

Training Manual on Quality Assessment of Food Products

Solid-not-fat is determined by using following expression. SNF = CLR + 0.21 fat + 0.66 4 Suppose CLR is = 28.0 and Fat% = 6% then. SNF = 28 + 0.21 x 6 + 0.66 4 = 7 + 1.26+0.66 SNF = 8.92% 2.3. Clot on Boiling Test (COB) Principle COB test will be positive if acidity is more than 0.2% Procedure Take about 5ml of well mixed sample in a test tube. Keep it in a water bath for 5 min., or rotate it almost horizontally on a spirit lamp so as to boil the milk. Interpretation Clotting of milk on the side of tube or at the bottom indicates poor keeping quality. Keeping quality Quality of milk COB should be ve i.e. no clot should form on boiling. COB + ve milk should be separated and not mixed with good milk. For good Natural Acidity of Milk :

Ten ml of milk is mixed well with as much amount of distilled water in a flask and the 1-2 drops of phenolphthalein indicator are added. Then N/9 NaOH is run down from a burette to the content is the flask until a light pink color appears. The amount of N/9 NaOH utilized is noted down. 1 ml of N/9 NaOH solution is equivalent to 0.01 g of lactic acid. Good quality milk has 0.12-0.15% lactic acid, sour milk has 0.15-0.20 lactic acid and curded milk has 0.7 to 2.0% lactic acid.

2.4. pH OF MILK USING pH PAPER: Certain indicators show change in colour with the change in pH. The pH paper or strips are impregnates with these indicators such as bromothymol blue (pH 6.0 to 7.6) and bromocresol purple (pH 5.2 to 6.8). pH papers in narrow range and wide range are available.
Training Manual on Quality Assessment of Food Products 33

Objectives : To study the freshness of milk. Reagents : pH ++paper strips Procedure


Take a small quantity of milk in the test tube. Dip the pH strip in the milk. Compare the colour changes with standard chart and note the pH.

Precaution The result with pH paper are not precise and for more precision pH meter is used. The pH strips should be stored in a glass bottle properly stoppered in dry conditions. Interpretation Normal milk pH is between 6.6-6.8. pH above 6.9 is indication of mastitic milk/late lactation milk. 2.5. Phosphate Test : This test is taken as an indicator of proper pasteurization. To determine whether a lot of milk is properly pasteurized or not. 10ml of the pasteurized milk sample is mixed with 1 ml. of p-nitrophenyl disdium. This is then kept at 37C temp. for 30 minutes and observed for appearance of yellow coloration. Under pasteurized milk give yellow color while properly pasteurized milk will give no coloration. 2.6. Alcohol Test : The alcohol test determines the susceptibility milk of coagulate due to developed acidity or unbalance salt. This test is of prime importance in milk to detect milk which has a tendency to curdle during processing sterilization or pasteurization. Procedure : Five ml of raw milk is mixed with 5ml of 8% absolute alcohol, if precipitation occurs then the alcohol test is + ve i.e. milk is least heat stable. Absence of any precipitation indicates appropriate heat stability of milk. 2.7. Methylene Blue Reduction (MBRT) : MBRT is one of the most important tests for quality assessment of milk. It is an indicator of shelf life or keeping quality of milk in addition of checking whether milk is properly pasteurized or not. To determine the test, 10ml milk is taken in a test tube and to it 1 ml of methylene blue dye is mixed. The content is heated and kept in a waterbath at a temp. of 37oC. Methylene blue dye is prepared in oxidized form. Bacteria Present in milk reduce this dye in a short time. So if blue colour in the test tube (dye+milk) is changed to white in short time, this shows that larger count of bacteria is still present in the milk which is attributed to improper pasteurization.

34

Training Manual on Quality Assessment of Food Products

2.8. Resazurin Reduction Test (RRT) This test is similar to the Methylene blue test, but it uses the indicator resazurin to measure the bacteriological quality of milk. The colour of resazurin at the normal pH of milk is blue. This compound is reduced to resorufin, which is pink, the colour changing gradually during the reduction process. The test milk is added to a screw capped vial plus resazurin to give a concentration of about 1 part of dye in 1,80,000 parts of milk. Standard tablets of resazurin are available, one tablet dissolved in 50 ml of boiled, cooled distilled water make 0.005% solution which can be directly used in the test. The tubes are then incubated in a water bath at 37oC. After the samplus reach this temperature, they are gently inverted three times and returned to the bath, then the time of incubation begins. For 1 hour and 10 mts RRT tests samples are compared with control tubes (milk without dye and incubated at 37oC) is a lovibond comparator with Resazurin disc. The disc will have 6 disc (Starting 06 with colours ranging from blue, and shades of purple, lavender and pink). The disc number matching is recorded and the quality of milk is graded as follows. 1 Hour RRT test Disc No 4.5 (or) 6 3 - 1 0.5 & 0 10 Mts RRT Test Disc No. 4.5 or 6 3 -1 0.5 and 0 Quality Satisfactory Doubtful, requires further examination Unsatisfactory Quality Good Fair Poor

2.9.DIRECT MICROSCOPIC COUNT (DMC Test) Direct microscopic count (DMC) is one of the several methods used in quality control laboratories for direct enumeration of micro organisms in milk sample. It consists of examining fixed and stained smears of a known volume of milk and milk products under a compound micro scope. This method provides a rapid indication of quality of milk or liquid milk products. A small quantity (0.01 ml) of the sample is spread over the outlines area of one cm square (100 mm2) on a grease proof microscope slide with the help of a breeds pipette. After making a uniform smear, it is air dried, fixed, stained with new-mans stain and then examined under the microscope. The number of organisms per field is counted and average number per field is determined after examining at least 10-20 fields. Total number of organisms (viable as well as non viable) per ml are then calculated by multiplying the average number of organisms per field by the microscopic factor.

Training Manual on Quality Assessment of Food Products

35

For determining the microscopic factor (MF) of a given compound microscope, the following formula is used. MF = 100 x 100 r2 Where r is equal to radius of the microscopic field. (pi) is a constant having a value of 3.14. In this formula in order to convert area of one field from Sq. mm to sq. cm field area in Sq mm has been divided by hundred. The number of such fields to be counted depends upon the average number of organisms per field as given below.

The average number of organism per field multiplied by the MF yields the number of organisms per ml of milk product. It is better to count clumps instead of individuals cells because clump count agrees most with SPC. Results Interpretation Count / Ml Less than 5,00,000 5,00,000 4,000,000 4,000,0000 20,000000 Over 20,000,000 Quality Good Fair Poor Very Poor

2.10. STANDARD PLATE COUNT The standard plate count or pour plate method is used for estimating the viable micro organisms in milk and milk products. In view of a wide range of bacterial population in dairy products, their number can be counted only by making appropriate dilutions. An aliquot of 0.1 ml or 1 ml of the diluted samples is poured in sterilized plates and mixed with liquefied sterilized agar medium. After solidification of agar, the plates are incubated at a specific temperature and for suitable period of time depending on the type of bacteria being suspected in the food sample. After incubation, bacterial cells grows in to distinct and isolated colonies (each colony develops from a single bacterial cells) which can be counted with the help of a colony counter. The plates with 30 300 colonies are selected for counting to obtain plate counts or colony forming units (cfu) per ml or g of the product. In order to calculate the total number of viable bacteria / g or ml of the sample, the number of the colonies developed on each plate are multiplied by the dilution factor.

36

Training Manual on Quality Assessment of Food Products

The dilutions will be 1 : 10, 1 : 1000, 1 : 10000, 1 : 1,00000, 1 : 10,00000 etc. done as shown in the figure.

Fig. 5.3 Protocol for preparing dilutions of a milk sample, indicating volumes to be added to dilution blanks and petridishes INTREPRETATION OF RESULTS Count / Ml Quality / Grade

Less than 2,00,000 2,00,000 1 million 1 5 millions Over 5 million 2.3.11. Coliform Test:

Very good Good Fair poor

The members of the coliform group of bacteria eg. Escherichia and aerobacter aerogenes are commonly found in dairy products, produced and handled under insanitary conditions. Their presence in milk and milk products is indicative of possible faecal contamination although some species (Aerobacter aerogenes) may be derived from feeding materials and soil. The test for coliform organisms is based on the principle that the members of this group are capable of producing acid and gas from lactose in the presence of bile salt. A small amount of milk (1.0, 0.1 or 0.01 ml) is added to liquid or solid media containing lactose and bile salt with a suitable indicator. Production of acid and gas in liquid media and appearance of typical colonies of coliform on the plates is taken as evidence of coliform contamination. A few other bacteria such as those belonging to the genus clostridium and gencus bacillus and certain yeasts also produce acid and gas under these conditions giving rise to false positives. However even these organisms are undesirable in milk and their interference with the test therefore is not considered to be of much significance. Hence the test commonly employed to detect the presence of coliform bacteria in milk is called presumptive test and in cases of doubt the completed test in considered to confirm the presence of coliform. Liquid Media test : Transfer 1 ml portion of milk and its dilutions (1 / 10 and 1/ 100) into macconkeys broth tubes in triplicate. Incubate the tubes for 24 hours at 37oC and observe for acid and gas production.
Training Manual on Quality Assessment of Food Products 37

The production of acid is indicated by change of colour of medium from purple to yellow in the case of bromocresol purple and orange to pink in the case of andrades indicator. Production of gas is observed in the Durhams tubes which may be partially or completely filled with gas. If no changes is observed incubate for another period of 24 hours and record the observation. Solid Media Test Incubate 1 ml portion of the required dilutions into sterile petridishes (in duplicate). Add to each plate 10 -15 ml of Macconkeys agar previously melted and cooled to 45oC. Mix the content thoroughly by tilting and rotating the plates. Allow the agar to solidify. Pour additional layer (3 4 ml) of the medium completely over the surface of the solidified medium.. Invert and incubate the plates at 37oC for 24 hours. After incubation examine for typical colonies of coliform bacteria. Presence of dark red colonies measuring at least 0.5 mm in diameter constitute a positive test. Count such colonies only and express the results as coliform count per ml of milk, 2.3.12. Yeast & Mould For certain dairy products the yeasts and moulds count is used as an index of proper plant sanitation and high quality raw products. Yeasts and moulds counts can be made by using potatodextrose agar or malt agar with a pH adjusted to 3.5 + 0.1. At this pH bacterial growth is inhibited although most yeasts and moulds are uninhibited of owing their preference for an acid reaction. The pH is adjusted with a predetermined amount of sterile 10% tartaric acid after the medium is melted and tempered and then plates are poured in the usual manner explained under SPC method. The medium should not be acified before sterilization or melting for the acid will hydrolyse the agar and destroy its ability to solidify. Extended holding of the acidified melted agar will prove undesirable for the same reason. The plates are incubated at 21oC or 25oC. for 5 days and the count is reported as yeasts and mould plate count per ml of milk or butter. When examining butter, one should place a quantity of the product in a sterile jar and should warm this in a bath at 40oC until the butter melts. Then 1:10 dilution is prepared by adding 11 ml of the melted butter to a 99 ml of water blank from which after dilutions can be made. It is well to have all glassware and dilution blank tempered to 45oC, until just before use to facilitate the handling of the sample and to prevent any solidification. The pipeting of diluted sample should be done immediately subsequent to shaking while the fat droplets are evenly distributed. This will aid in preventing errors caused by the coalescing of the fat and by uneven distribution of organisms adhering to the fat droplets. 2.1. ADULTRANTS IN MILK AND MILK PRODUCTS Adultration of milk may be defined as addition of any material to the milk, or removal of any constituent of milk. As per PFA adultration of milk is not allowed and it is punishable with fine and imprisonment. The common adulterants in milk are 1. 2. 3.
38

Addition of water Addition of starch / cereal flour Addition of cane sugar


Training Manual on Quality Assessment of Food Products

4. 5. 6. 7.

Addition of urea Addition of skim milk powder Addition of Vanaspati Addition of Formalin

8. Addition of Gelatin 9. Addition of Ammonium sulphate

10. Addition of glucose Detection of Adultrants in milk 1. Added Water: The presence of water can be by putting a drop of milk on a polished slanting surface. The drop of pure milk either or flows lowly leaving a white trail behind it, where as milk adulterated with water will flow immediately without leaving a mark. 2. Addition of starch / Cereal flour

Take 3 ml of well mixed sample of milk in a test tube Boil the milk over a bunsen burner Cool and add one drop of 1 percent Iodine solution and observe for colour change.

Iodine solution gives intense blue colour with starch due to formation of an unstable complex starch iodo compound. So development of blue colour indicates adulteration of milk with starch / cereal flour. 3. Addition of Cane Sugar

Take 10 ml of milk in a test tube Add 1 ml of concentrated hydro chloric acid and mix Add 0.1 g of resorcinol powder and mix thoroughly Place the test tube in a boiling water bath for 5 minutes and observe for colour

Red colour obtained with resorcinol indicates adultration of milk with cane sugar. 4. Addition of Urea

Take 5 ml of milk sample in 50 ml of conical flask. Add 5 ml of sodium acetate buffer or 24% Trichloroacetic acid solution and heat for 3 minutes in boiling water bath (no heating if Trichloroacetic acid is used). Filter the precipitates through a what man no 42. Filter paper and collect 1 ml of filtrate in a test tube.

Training Manual on Quality Assessment of Food Products

39

Add one ml of sodium hydroxide solution (2% solution) to the filtrate, followed by 0.5 ml of sodium hypochloride solution (2% solution), mix thoroughly and finally add 0.5 ml of 5% (W / V) phenol solution and observe.

A characteristic blue or bluish green colour in the filtrate from the milk with extraneous urea indicate the presence of urea. Colourless indicates no urea added. This will detect even 0.1 percent of urea addition. 5. Addition of skim milk powder

Take 50 ml of milk in each of two centrifuge tubes and balance properly in the centrifuge. Centrifuge at 3000 RPM for 30 mts. Decant the supernatant liquid carefully. Dissolve the residue in 2.5 ml of concentrated nitric acid. Dilute the solution with 5 ml of water. Add 2.5 ml of liquid ammonia and observe for colour development.

Skim milk powder being highly proteinacious in nature gives orange colour with nitric acid, while unadulterated milk being low in protein content gives only a yellow colour. 6. Addition of Vanaspati Take 3 ml of milk in a test tube. Add 10 drops of hydrochloric acid. Mix up one teaspoonful of sugar. After 5 minute, examine the mixture. The red colouration indicates the presence of vanaspati in the milk. 7. Addition of Formalin Take 10 ml of milk in a tests tube and add 5 ml of con Sulphuric acid from the sides of the wall without shaking. If a violet or blue ring appears at the intersection of two layers then it shows presence of formalin. 8. Addition of Gelatin

Take 10 ml of milk in a test tube Add an equal amount of acid mercuric nitrate solution (mercury is dissolved in twice its weight of nitric acid of sp. G. 1.422. Before use this solution is diluted with distilled water to 25 times its volumes. Shake and add 20 ml of distilled water, shake again and allow to stand. Filter after 5 minutes. Add to a part of the filtrate an equal volume of picric acid reagent (Saturated solution of picric acid solution) and observe.

White cloudiness shows the presence of gelatin in milk. Yellow precipitate indicates a large amount of gelatin added. Transparent yellow solution indicates absence of gelatin.
40 Training Manual on Quality Assessment of Food Products

9. Addition of Ammonium sulphate Take 1 ml of milk in a test tube.


Add 0.5 ml of sodium hydroxide (2%) solution and 0.5 ml of sodium hypochlorite solution (2%) and mix thoroughly. To the solution add 0.5 ml of phenol solution (5%) and heat for 20 seconds in a boiling water bath, and observe.

A bluish colour immediately forms, which turns deep blue after wards, in the sample of milk having added ammonium sulphate. In case of pure milk only a salmon pink colour forms which gradually changes to bluish in course of about 2 hours, even 0.1 % addition of ammonium sulphate can be detected by this method. 10. Addition of Glucose

Take 1 ml of milk sample in a test tube. Add 1 ml of Bar foeds reagent. Heat the mixture for 3 minutes in boiling water bath and cool for 3 mts under tap water. Add one ml of phosphomolybdic acid reagent to the turbid solution and observe.

Immediate formation of deep blue colour indicates the presence of extraneous glucose, which is stable for 24 hours. In case of pure milk only faint bluish colour due to diluted barfoeds reagent appears. By this methods as low as 0.05 % extraneous glucose in milk can be detected. 10. Addition of Detergent Shake 5 10 ml of sample with an equal amount of water lather indicates presence of detergent. Detection of Adultrants in milk products 1. Sweet curd Vanaspati Take 1 teaspoon full of curd in a test tube. Add 10 drops of hydrochloric acid. Mix up the contents shaking the test tube gently. After 5 minutes, examine the mixture. The red colouration indicates the presence of vanaspati in curd. 2. Rabri Blotting paper Take a teaspoon of rabri in a test tube. Add 3 ml of hydrochloric acid and add 3 ml of distilled water. Stir the contents with a glass rod. Remove the rod and examine. Presence of fine fibres to the glass rod will indicate the presence of blotting paper in rabri. 3. Khoa and its products - Starch Boil a small quantity of sample with some water, cool and add a few drops of iodine solution. Formation of blue colour indicates the presence of starch.

Training Manual on Quality Assessment of Food Products

41

4. Paneer or Chana Starch Boil a small quantity of sample with some water, cool and add a few drops of iodine solution. Formation of blue colour indicates the presence of starch. 5. Ghee a. Vanaspathy or margarine Take about 1 teaspoon full of melted sample of ghee with equal quantity of concentrated hydrochloric acid in a stoppered test tube and add to it a pinch of sugar. Shake for 1 minute and let it for five minutes. Appearance of crimson colour in lower (acid) of vanaspati or margarine. b. Mashed potatoes, Sweet potatoes and other starches The presence of mashed potatoes or sweet potatoes in a sample of ghee can easily be detected by adding few drops of iodine, which is brownish in colour turns to be blue if mashed potatoes / sweet potatoes/other starches are present. 6. Butter a. Vanaspathy or margarine Take about 1 teaspoon full of melted sample of ghee with equal quantity of concentrated hydrochloric acid in a stoppered test tube and add to it a pinch of sugar. Shake for 1 minute and let it for five minutes. Appearance of crimson colour in lower (acid) of vanaspati or margarine. b. Mashed potatoes, Sweet potatoes and other starches The presence of mashed potatoes or sweet potatoes in butter can easily be detected by adding few drops of iodine( which is brownish in colour), turns to be blue. 7. Ghee, cottage cheese, condensed milk, Khoa and milk powder etc., - Coal tar dyes Add 5 ml of diluted sulphuric acid or concentrated hydrochloric acid to 1 teaspoon full of melted sample in a test tube. Shake well. Pink colour (in case of H2SO4) or crimson colour (in case of HCL) indicates coal tar dyes. If HCL does not give colour, dilute with water to get the colour. 2.2. DETECTION OF PRESERVATIVES IN MILK Micro organisms are susceptible to the action of chemicals which either check their growth or destroy the organisms and then keep the milk for a longer time. 1. Boric Acid or Borax
42

Take 5 ml of milk in a test tube. Add 1 ml of concentrated hydrochloric acid and mix well. Dip a strip of turmeric paper in the acidified milk. Dry the filter paper immediately and note the change in colour. Turmeric paper turns red if boric acid or its salts are present.
Training Manual on Quality Assessment of Food Products

2. Carbonates / Bicarbonates

Take 10 ml of milk in a test tube. Add 10 ml of alcohol and shake well. Add 3 drips of aqueous solution of rosalic acid (1%) Mix well and observe the change of colour.

Rose red colour indicates presence of carbonate / bicarbonate in the milk. Only brownish colour indicates absence of carbonate / bicarbonate. 3. Formalin There are two tests a) Hehnes Test

Take 10 ml of milk in a test tube Add 0.5 ml of 1% ferric chloride solution. Add carefully about 5 ml of concentrated sulphuric acid down the side of the test tube in such a way that it forms a separate layer at the bottom without mixing with milk. Observe the colour of the ring formed at the junction of the two liquids.

b) Leech Test

Take 5 ml of milk in a test tube Add to it equal volume of concentrate hydrochloric acid containing 1 ml 10% ferric chloride solution to each 500 ml of the acid. Heat over a flame for 5 minutes. Rotate the tube to break up the curd and observe the colour. Violet colour indicate presence of formaldehyde.

4. Hydrogen Peroxide

Take 10 ml of a sample of milk in a test tube. Add 2 drops of paraphenylene diamine hydrochloride solution mix thoroughly and observe.

Development of an intense blue colour indicates presence of hydrogen peroxide. 5. Salicylic Acid Mercuric nitrate is added to the milk and milk is filtered. If much salicylic acid is present the filtrate attains a red colour after some time. 6. Benzoic Acid About 20 gms of milk is treated with equal volume of concentrated hydrochloric acid until the curd dissolves. It is now allowed to cool. About 25 ml of a mixture of either and petroleum ether is
Training Manual on Quality Assessment of Food Products 43

added to the mixture of milk and hydrochloric acid and is shaken. The ether layer separation and gives a precipitate with a drop of ammonium hydroxide in the presence of benzoic acid. 7. - Naphthol Milk is extracted with chloroform and heated with potassium hydroxide for few mts. If a deep blue colour appears it indicates the presence of - naphthol. 3.1.CREAM 3.1.1. Fat by Gerber method Procedure a. Mix the sample by carefully stirring without causing frothing or churning. If the cream is very thick, warm it to 30o C.

b. Weigh 5 gm of cream in the cream butyrometer (0 70% range) by keeping the butyrometer in a conical flask. c. Add about 18 -20 ml of 50% Gerber acid (freshly prepared by adding equal volumes of sulphuric acid and distilled water). Take care that there is space for 1 ml amyl alchol are added. After covering it with a cork the tube is taken in centrifuge for 5 mts. Then the fat percentage is calculated.

d. Proceed as in the case of milk. e. Record the fat %.

One more method To the butyrometer tube 10 ml Gerbers acid and 3 ml of the given cream is pipette out into it. Then 8.2 ml of distilled water and 1 ml of amyl alcohol are added. After covering it with a cork the tube is taken in centrifuge for 5 mts. Then the fat percentage is calculated. For thin cream = (B.R 4) - 0.8 = % fat Thick cream = (B.R 4) 0.8 2 = % fat

(Diluted with equal quantity of water) 3.1.2. SNF SNF % = 100 Fat % in cream _______________________ 11 3.1.3. Acidity Procedure a. Mix the sample by carefully stirring without causing frothing or churning. If the cream is very thick, warm it to 30 - 40p c and then mix it.
Training Manual on Quality Assessment of Food Products

44

b. Pipette out 10ml or weigh 10 gm if it is too viscous into a beaker. c. Add minimum amount of distilled water to make the sample sufficiently liquid for titration.

d. Proceed as in milk. % Acidity= 9VN ______________ W V- Volume of 0.1N NaOH N- Normality of 0.1N NaOH W-Weight of cream 3.1.4 Phosphatase Test: Procedure: i) Transfer 5ml of buffer substrate solution in to a test tube. Bring the temperature to 37C. ii) Add 1 ml of cream to the solution. ii) Incubate at 37C in a water bath for 5-10 minutes. iv) Prepare one blank from boiled cream of same sample. Conclusion: Yellow colour indicates under pasteurization. Compare the colour with that of blank. Buffer Solutions: 3.5g of anhydrous AR Sodium Carbonate and 1.5g AR Sodium bicarbonate dissolved in water and made upto 1ltr. Substrate: P.Nitro-Phenyl-Disodium Orthophosphate Buffer Substrate: Transfer 0.15g of the substrate in 100 ml flask, make upto the mark with buffer solution. The solution should be practically colourless and should not be stored for longer period (1 week). 3.2 BUTTER: According to PFA Rules (1976), table or creamery butter should contain not less than 80% fat, not more than 1.5% curd and not more than 3.0% common salt.

Training Manual on Quality Assessment of Food Products

45

3.2.1. MOISTURE (GRAVIMETRIC METHOD) Procedure a) Take clean dry flat bottom aluminum dish and weigh. b)Take 10g of sample into the dish and weigh it. c) Put the dish on steam water bath or on hot plate with frequent stirring until no moisture is seen at the bottom of the dish and curd particles turn slightly brown in color.

d) Wipe the bottom of the dish and keep in an oven at 100+10C for 90 min. e) f) Cool the dish in a dessicator and weigh. Repeat the process of heating (30min.) cooling, weighing until the difference between two consecutive weighting does not exceed 0.1mg.

Interpretation Moisture % should not exceed 16%. 3.2.2. SALT Procedure a) Weigh 10g of butter in a beaker. b) Add hot distilled water to melt the butter and transfer it into a separating funnel without disturbing the top fat layer, run down the water layer in a 250ml volumetric flask. c) Wash repeatedly the fat left in the separating funnel thrice with small quantities of hot distilled water and collect the washings.

d) Cool the contents to room temperature and make up voloume to 250ml mark with distilled water. e) Take 25ml of this sol and add 1ml potassium chromate indicator and titrate against 0.1N silver nitrate until a brownish colour persists for min.

Interpretation: Salt % = 5.85 x N x B/A NB ANormality of AgNO3 Vol. of AgNO3 used Wt. of butter i.e. 10g

3.2.3. OVER RUN


The Weight of butter obtained from a given lot of cream exceeds the amount of fat in cream. The amount of butter which exceeds the fat present in cream is called over run.

46

Training Manual on Quality Assessment of Food Products

Over run may be defined as the increase in the amount of butter made from a given amount of fat. It is usually expressed in percentage. Over run is caused by the presence of Moisture, curd particles and salt in butter. It is a source of profit to the manufacture. % Over run = B-F 100 ________ F

B- Butter made (kg) F FAT in Cream (kg) 3.3. GHEE Standards and Specification of Ghee Moisture max F.F.A. Taste Residue 3.3.1. MOISTURE Procedure a) Weigh a dried and cooled moisture dish. b) Weigh 10g of sample in this dish. c) Keep the dish in hot air oven at 105+1oC for 1 hr. 0.25% 0.5% Pleasant Absent

d) Take out dish from oven and cool, weigh it. e) f) Keep the dish in the oven for hr., cool and weigh it. Repeat heating, cooling and weighing until the loss of wt. between two consecutive weightings does not exceed mg.

Interpretation Weight of dried sample 100 _________________ Moisture % by wt. = Sample weight

Moisture should not more than 0.3%.


Training Manual on Quality Assessment of Food Products 47

3.3.2. FREE FATTY ACID (AS OLETIC ACID) Procedure a) Weigh 10g of sample in a 250ml conical flask. b) Add 50ml of neutralized alcohol in the flask and mix the contents. c) Digest the mixture over a hot water bath at 50oC for 15 min by continuously agitating the flask.

d) Titrate immediately with 0.1N Sodium hydroxide using 1ml of phenolphthalein indicator. e) f) The end point of the titratin is reached when the addition of a single drop produce a slight, but definite change, persisting for 15 sec. Read the volume of Sod. Hydroxide used during titration (v).

Interpretation Free fatty acid (%oleic acid) = 2.82 V/A A Wt. of Sample taken.

Free fatty acid should not be more than 1.2%. 3.3.3. MINERAL OIL TEST Procedure Take 50ml of ghee. Boil it. Add 22ml of alcoholic KOH and 25ml boiled distilled water. Wait for a minute. Interpretation If ppt. occur then adultration of mineral oil but if clear or transparent solution it indicates no adultration of mineral oil. 3.3.4. BUTYRO REFRACTOMETER TEST (B.R.TEST) It ranges between 40-43. Procedure For testing of sample by Butyro Refractometer, the apparatus is maintained at 40oC by circulating water at least 10min. Now oil/Fat to be tested is put on the glass of B.R. and it is covered now reading is observed on the scale. That reading is B.R. value of given sample. B.R. Value of same imp. Oil/Fat Sr. No. 1. 2. 3.
48

Oil Fat Palm Oil Parachute Coconut Oil Dalda Ghee

B.R. Value 47 34 51
Training Manual on Quality Assessment of Food Products

4. 5. 6. 7.

Soyabean Oil Mustard Oil Groundnut Oil Sunflower Oil

62 60 65.5 62

3.4. STERILISED FLAVOURED MILK 3.4.1. TURBIDITY a. Weigh 4 gm of Ammonium sulphate with a graduated cylinder and transfer it to the same flask.

b. Measure 20 ml of milk sample with graduated cylinder and transfer it to the same flask. c. Shake well for 1 min to completely dissolve the ammonium sulphate. Set it aside for 10 min.

d. Filter through a filter paper and collected 5 ml of clear filtrate in a test tube. e. Keep the test tube to a beaker of cold water. Examine it for turbidity.

Conclusion No sigh of turbidity indicates satisfactory sterilization A. Fat by Gerber method B. SNF by lactometer (including added sugar) 3.5. CHEESE/PANEER 3.5.1. Fat Procedure i) Weigh accurately about 3g of finely devided cheese samples into the cheese butyrometer.

ii) Add 10 ml of gerbers acid, 10ml of distilled water and 1 ml of amyl alcohol. iii) Close the butyrometer with the lock stopper and shake well till all the contents are mixed well. iv) Place the butyrometer in a water bath at 65C2C. v) Shake well periodically until the solution of cheese is homogeneous. vi) Centrifuge at 1200 rpm for 5 minutes. vii) Read the percentage of fat by adjusting the fat column within the scale of butyrometer. Interpretation According to PFA standards, hard variety of cheeses should contain not less than 42% milk fat on dry matter basis. The processed cheese should contain not less than 40% milk fat on dry matter basis.
Training Manual on Quality Assessment of Food Products 49

3.5.2. Moisture Procedure: a) Weigh a dried and cooled moisture dish. b) Weigh 2-3g of cheese sample in this dish. c) Keep the dish in hot air oven at 70oC for 8 hr.

d) Take out dish from oven and cool, weigh it. e) f) Keep the dish in the oven for hr., cool and weigh it. Repeat heating, cooling and weighing until the loss of wt. between two consecutive weightings does not exceed mg. Weight of dried sample 100 ______________________ Moisture % by wt. = Interpretation According to PFA standards, hard variety of cheeses should contain not less than 43% moisture and the processed cheese should contain not less than 47% moisture. 3.5.3. Acidity Procedure 1. 2. 3. 4. Weigh accurately 2 gm of well mixed cheese in a conical flask. Add 20 ml of distilled water and make a fine paste with a glass rod. Add 2 drops of 0.5 % phenolphthalein solution. Titrate against N/10 sodium hydroxide solution till a faint pink colour persists. Sample weight

Calculation 1 ml of N/10 Sodium hydroxide = 0.009 gm of lactic acid. 0.009 V ml of lactic acid. 0.009 V _____ W 3.4.4. Salt a. Weigh accurately 2 gm of cheese in a conical flask.

Then V ml. of N/10 Sodium hydroxide = % acidity in the cheese sample =

b. Add 20 ml of distilled water and make up a paste. c.


50

Add 10 ml of nitric acid.


Training Manual on Quality Assessment of Food Products

d. Add 12.5 ml of N/10 silver nitrate solution. Digest on stove. e. f. Add 50 ml of distilled water again and 2 ml of ferric alum indicator. Titrate against 0.1 N Potassium thiocyanate solution till brick red colour persists (v2). (11 gm of KSCN in 1 it. Water gives 0.1 N KSCN).

g. Repeat with blank (v 1) Salt % = (v1 v2) 0.292 V1 V2 = Blank reading = Volume of KSCN with sample

3.5. ICE CREAM 3.5.1. Fat Procedure 1. 2. 3. 4. Weigh carefully 5 gm of melted sample into a butyrometer. Add 6 ml of hot water, 10 ml of Gerbers acid and 1 ml of amyl alcohol on to the butyrometer. Insert the stopper. Shake the contents and centrifuge for 5 minutes at 1100 rpm. Keep the butyrometer in a water bath at 60C for 5 minutes. Read the fat content.

Interpretation as per ISI standards The ice cream should contain a minimum of 10% milk fat. Softy Ice cream The average fat percentage in a softy ice cream is 3-6% 3.5.2.Titratable Acidity Procedure 1. 2. 3. 4. Weigh 20 gm of the ice cream in a porcelain dish. Add 50 ml of distilled as water. Add 1 ml phenolphthalein indicator. Titrate against standard sodium hydroxide in the burette till a pink colour is formed and remains for 10 15 seconds. Note the burette reading as V1.

Training Manual on Quality Assessment of Food Products

51

Calculation %acidity = 9 V1 N1 _________ V2 V1 Volume in ml of 0.1N NaOH required for titration. N1 Normality of the standard NaOH solution used V2 Weight in g of the product taken Interpretation as per ISI standards The acidity of Ice cream should not exceed 0.25% (as lactic acid) 3.5.3. Over run Over run is defined as the volume of ice cream obtained in excess of the volume of the mix. This increased volume is mainly composed of the air incorporated during the freezing process. The amount of air which is incorporated depends upon the composition of the mix and the way it is processed. Calculation % Over run= Volume of ice cream Volume of mix100 __________________________ Volume of mix Interpretation The desirable percentages of over run in different types of ice cream or given as follows: Products Ice cream(Packaged) Ice cream(Bulk) Softy Ice cream(softy) 3.6. Condensed Milk 3.6.1. Fat: Procedure

% over run 70-80 90-100 30-50

Weigh carefully 25 gm of the homogeneous sample of Condensed Milk in a clean beaker. Add 50 ml of distilled water and mix thoroughly Trasfer reconstituted milk into a 100 ml of volumetric flask. Wash the beaker thrise with 100 ml of distilled water and transfer in to the volumetric flask.
Training Manual on Quality Assessment of Food Products

52

Make upto 1oo ml mark with distilled water and mix the contents well. Take 10 ml gerbers acid in to the butyrometer. Add 11 ml of reconstituted diluted milk and 1 ml of amyl alcohol Stopper the butyrometer, invert the butyrometer 2-3 times and mix the contents. Place the butyrometer in the water bath at 65C2C for 5 minutes. Keep the butyrometer in a water again bath for 5 minutes and remove. Centrifuge for 5 minutes at 1200 rpm. Adjust the fat column with in the scale of butyrometer and take the reading.

Calculation Fat %= butyrometer reading 100 __________________________ Weight of condensed milk Interpretation as per ISI standards Condensed milk should contain not less than 9% milk fat. Skim milk and sweetened condensed milk should contain not more than 0.5%milk fat. 3.6.2. Titratable Acidity Procedure 1. 2. 3. 4. 5. 6. Weigh 10gm of condensed milk in a suitable dish. Add 30 ml of luke gram of water and 1 ml phenolphthalein indicator solution. Shake well and titrate against standard sodium hydroxide solution. Stir vigorously throughout. Complete the titration in 20 secounds. Keep in another disk about 10 g of sample diluted with 30 ml luke warm water as a blank for comparison of colour. The persistence of a slight pinkish tinge for 30 sec, indicates the end point. The titration shall be preferably made in normal light.

Calculation Titratable acidity = 9 V1 N1 ________________ V2 V1 Volume in ml of 0.1N NaOH required for titration. N1 Normality of the standard NaOH solution used V2 Weight in g of the product taken
Training Manual on Quality Assessment of Food Products 53

Interpretation as per ISI standards Acidity of Condensed milk and Skim sweetened milk may contain upto a maximum of about 0.35% (as lactic acid). 3.7. Dried Milk 3.7.1. Moisture Procedure a. Weigh a clean dry dish (W1).

b. Transfer to the dish 10 gm of milk powder sample and weigh accurately (W2). c. Place the dish in an oven at 102C for 3 hours or (125C for 15 min).

d. Remove it from oven and cool it in a desiccators and weigh (W3). e. Repeat it till a constant weight in two successive weightments is reached. Moisture = W2 W3 100 ________________ W2 W1 3.7.2. Fat by Gerber method Procedure a. Weigh accurately 1.68 gm of powder in a beaker.

b. Dissolve it in 10 ml of water slowly and mix it well. c. Add Gerber acid, amyl alcohol and proceed in milk test.

d. Note fat % in the butyrometer. Fat % in powder = Fat % butyrometer 20 ________________ 3 3.7.3. Total solids (T.S) T.S. = 100 Moisture % SNF = T.S Fat % 3.7.4. Titratable Acidity Procedure i) Weigh accurately about 1g of the sample in to each of two porcelain dishes.

54

Training Manual on Quality Assessment of Food Products

ii) Add 10 ml of boiling water to each dish and stir with the flat end of a glass rod until a perfectly smooth liquid is obtained and cool to room temperature. iii) Use the contents of one dish as a blank by stirring in 2 ml of rosailine acetate. iv) Add 1 ml of phenolphthalein indicator solution to the other dish followed by the addition of standard sodium hydroxide (NaOH) solution in drops from the burette until the colour matches the pink taint of the blank. v) Stir the contents vigorously. The time taken for the complete titration shall not exceed 20 seconds. Calculation Titratable Acidity = 9 V1 N1 _________ V2 V1 Volume in ml of 0.1N NaOH required for titration. N1 Normality of the standard NaOH solution used V2 Weight in g of the product taken 3.7.5. Solubility Index Procedure Reconstitution Add 14 g of the sample to 100 ml of distilled water at a temperature of 24C in the mixing jar. Place the jar in the mixer and stir for exactly 90 seconds. Allow the sample to stand until the foam has separated sufficiently to permit its complete removal by a spoon. The period of standing after mixing should not be more than 15 minutes. After removal of the foam, stir the sample thoroughly with a spoon for 5 seconds. Removal of cream and soluble fraction Fill up the centrifuge tube immediately with the reconstituted milk to the 50 ml mark. centrifuge the tube for 5 minutes, immediately siphon off the transparent liquid leaving about 5 ml above the sediment level, taking care not to disturb the sediment layer. Add about 25 ml of distilled water at a temperature of 24C. Invert and shake to mix the contents thoroughly. Again centrifuge for 5 minutes. Determination of Solubility Index Hold the tube in vertical position with the upper level of the sediment in level with the eye and read the ml of sediment in the tube to the nearest graduated scale division. The sediment is easily distinguished when the tube is held between the eye and an illuminated light source in the background. Calculation Report the solubility index as the milliliters of sediment in the tube.

Training Manual on Quality Assessment of Food Products

55

Interpretation as per ISI standards Milk Powder Whole milk and Skim milk powder a. Roller dried powder b. Spray dried powder 3.7.6. Solubility Percentage Procedure Reconstitution Weigh accurately about 4g of the material into 50 ml boiling tube. Add 32 ml of water at 50C. Cork the tube and shake for 10 seconds. Place the tube in a water bath at 50C for 5 minutes and shake the tube for 1 minute. Removal of Fat Fill up the brim of a centrifuge tube with the reconstituted milk and centrifuge for 10 minutes at 2000 rpm. Cool in a refrigerator or in ice until the fat becomes solid and forms a cake, taking care that milk does not freeze. Remove the fat layer with a little milk as possible by running a needle around the cake of the fat and then remove it. Warm the milk at 27C. Break up the deposit with the rod or wire. Cork the tube and shake well until the liquid appears to be homogeneous. 3.7.7. Total Solids Procedure i) Transfer about 2 ml of the homogeneous liquid to a previously weighed and dried aluminium dish (No.1). 15.0 2.0 Solubility Index (Max ml)

ii) Weigh the dish with the lid on and place it aside. iii) Centrifuge the tube again for 10 minutes. iv) Pipette about 2 ml of the upper layer of the supernatant liquid without disturbing the sediment into another aluminium dish (No.2).. Cover the dish and weigh. Calculation Solubility percent by weight = W4 W1100 __________ W3W2 Where, W1 - Weight in grams of total solids in dish no.2 W2 - Weight in grams of the liquid taken immediately after removal of fat in dish no.1
56 Training Manual on Quality Assessment of Food Products

W3 - Weight in grams of the supernatant liquid taken dish No.2 W4 - Weight in grams of total solids in dish no.1 Interpretation as per ISI standards Milk Powder Whole milk and Skim milk powder a. Roller dried powder b. Spray dried powder 3.8. Cultured Milk products 3.8.1. Fat Procedure

Solubility % wt (Max)

85.0 ml 98.5 ml

Weigh 100 g of sample in a beaker. Add 5 ml of strong ammonia to the weighed sample and shake well to make it homogeneous. Take 10 ml gerbers sulphuric acid in to the butyrometer. Pipette out 10.75 ml of the prepared sample and transfer in to the butyrometer carefully without allowing to mix with the acid. Add 1 ml of amyl alcohol. Stopper the butyrometer, invert the butyrometer 2-3 times and mix the contents. Butyrometer with the contents is centrifuged for 5 minutes at 1200 rpm. Adjust the fat column with in the scale of butyrometer and take the reading.

Calculation % Fat =B.R+ (B.R Dilution Factor) B.R Butyrometer Reading Dilution Factor is 1/20 3.8.2. Acidity Procedure i) Weigh accurately about 10g of well mixed dahi in dish.

ii) Add 25 ml of distilled and heat to boiling. iii) Add 1 ml of phenolphthalein indicator. iv) Titrate against 0.1 N sodium hydroxide (NaOH) solution.
Training Manual on Quality Assessment of Food Products 57

v) The end point is the appearance of pink colour. vi) Note the titre value. vii) Repeat the experiment to get the concordant values. Calculation Titratable Acidity = 9 V1 N1 ____________ V2 V1 Volume in ml of 0.1N NaOH required for titration. N1 Normality of the standard NaOH solution used. V2 Weight in g of the product taken. Interpretation as per ISI standards Character Acidity, lactic acid (% wt) 3.9. Khoa/Channa 3.9.1. Fat Procedure i) Weigh accurately about 3g of finely devided cheese samples into the cheese butyrometer. Sweet dahi 0.70 Sour dahi 1.0

ii) Add 10 ml of gerbers acid, 10ml of distilled water and 1 ml of amyl alcohol. iii) Close the butyrometer with the lock stopper and shake well till all the contents are mixed well. iv) Place the butyrometer in a water bath at 65C2C. v) Shake well periodically until the solution of cheese is homogeneous. vi) Centrifuge at 1200 rpm for 5 minutes. vii) Read the percentage of fat by adjusting the fat column within the scale of butyrometer. Interpretation According to PFA standards, Khoa should contain not less than 20% milk fat in the finished product and the channa should contain not less than 50% milk fat of the dry matter. The skim milk channa should not contain more than 13% milk fat of the dry matter. 3.9.2. Moisture Procedure a) Weigh a dried and cooled porcelain dish. b) Weigh 2-3g of sample in the dish.
58 Training Manual on Quality Assessment of Food Products

c)

Keep the dish in hot air oven at 70oC for 8 hr.

d) Take out dish from oven and cool, weigh it. e) Repeat heating, cooling and weighing until the loss of wt. between two consecutive weightings does not exceed mg. Weight of dried sample ______________________ Moisture % by wt. = Interpretation According to PFA standards, the channa and skim milk channa should not contain more than 70% moisture. Sample weight 100

Training Manual on Quality Assessment of Food Products

59

BACTERIOLOGY OF WATER
Water is essential for our daily life. It is transparent, colourless, odourless and tasteless liquid. Water is used for drinking, cleaning, domestic purposes and in processing of dairy products ans other industries. Water that is free of disease producing micro-organisms and devoid of chemical substances deleterious to health is called potable water. The sanitary quality of water is of very great importance whether it is meant for drinking or for use in dairy industries. As a potential carrier of pathogenic micro- organisms, water can endanger health and life. The pathogens most frequently transmitted through water (if water is polluted with faecal matter, sewage or manure) are those which cause infections of the intestinal tract viz. typhoid and paratyphoid bacteria (Salmonella typhi and salmonella paratyphi), dysentery (bacillary - Shigella and amoebic), cholera bactria (Vibrio cholera) and enteric viruses (polio virus). Natural waters (well and tanks) may also be contaminated with a variety of micro-organisms derived from soil, vegetation and other resources. Mostly gram-negative bacteria such as Psuedomonas, Flavobacterium, Acinetobacter, Chromobacterium and few gram-positive organisms such as micrococci and bacilli are present in natural water. For assessing the sanitary condition of water, it is generally examined for the total bacterial content and for the incidence of coliform bacteria. These bacteria are typical intestinal organisms and their presence in water serves as an index of pollution from sevege or faecal matter. A series of tests can be used to demonstrate the presence of coliform as an indicator of faecal contamination in water supplies. Materials Sterile glass stoppered / screw capped bottles. Spirit lamp Cotton Ethyl alcohol Match box Sterile petriplates Sterile pipettes Dilution blanks (physiological saline) Standard plate count agar Water bath maintained at 450 to 500C. Procedure 1. 2. 3. While collecting sample from the tap, clean the tap, wipe with alcohol and flame the top (only to metal tops and not to plastic tops). Allow the water to run for one minute. Filed the sample bottle in one hand near the tap, remove the stopper with the other hand, flame the mouth of bottle and quickly bring the bottle below the running stream of water. When the bottle is nearly full, take it out quickly and close it with the stopper.
Training Manual on Quality Assessment of Food Products

60

4. 5. 6. 7. 8. 9.

Transport the bottle immediately to the laboratory and refrigerate it until required for analysis. Shake the water sample thoroughly by moving the bottle up and down 25 times. Prepare two serial dilutions 1:10 and 1:100 using dilution blanks, mix the dilutions thoroughly by rotating the tubes between the palms or in a vortex mixer. Transfer 1 ml each of 0, 1 and 2 dilution blanks to the marked SPC plates in 2 sets of duplicates. Add 15-20 ml of melted SPCA to petriplates maintained at 450C, mix thoroughly and add melted MacConkey agar to coliform plates. After solidification, incubate the plates for 24-48 hours. SPC I set: 370C (faecal organisms grow) SPC II set: 220C (plant organisms grow)

10. Count the selected plates and tabulate the results.

Inference

SPC @ 370C : 220C should be 1:10 (the ratio changes if faecal contaminant are more). The number of organisms from plant source will always be more in good quality water. The presumptive test is most commonly used for the detection of faecal contamination in water and evaluation of its sanitary quality. The production acid and gas in lactose broth in 24-48 hours is regarded as presumptive evidence of coliform contamination in water. The test is used to determine the most probable number (MPN) of coliform present in 100 ml water. A sample showing more than 2 coliform bacteria / 100 ml is considered unsatisfactory. As the coliform group included both faecal and non-faecol types of bacteria, it is necessary conduct confirmatory tests for the presence of faecal coliforms in water. Presumptive coliform test The presumptive coliform test is used to determine the gas producing lactose fermenters that are present in water sample. It is determined using MacConkeys broth tubes. For this, the most probable number (MPN) of coliform present in 100 ml of water can be roughly estimated using MPN table. Materials Sample of water MacConkeys broth single and double strength
Training Manual on Quality Assessment of Food Products 61

Durhams tubes, sterile pipette and test tubes Procedure


Transfer 10 ml of water sample to 5 tubes of double strength broth tube containing 10 ml of the broth (This becomes 1:2 dilution). Transfer 1 ml and 0.1 ml of water sample into 2 sets of 5 tubes respectively of single strength broth tubes, each tube containing 10 ml of the broth (This becomes 1st and 2nd dilution). There will be 3 sets of 5 tubes each containing 10 ml, 1 ml and 0.1 ml of the water sample respectively.

Incubate the tubes at 37C/24 hours. The tubes showing no change should be incubated further for another 24 hours. Examine the tubes and record the number of tubes in each set that shows change in colour (wine red to yellow) and gas production in durhams tubes. Determine the MPN by referring to MPN table (Refer: Appendisx - 2).

Confirmatory test for coliforms Once it has been established that gas producing lactose fermenters are present in water, the water sample is considered unsafe. However, gas formation may be due to non-coliforms such as Clostridium perferingens or yeasts. To confirm the presence of gram-negative lactose fermenters,
62 Training Manual on Quality Assessment of Food Products

Endo agar or EMB agar is untitled for selective enumeration from the presumptive positive tubes. Endo agar contain a fuchsin sulphite indicator, which differentiate lactose fermenters. Coliform colonies and the surrounding medium appears red on Endo agar. Eacheiehia coli colonies are >0.5 mm in diameter with dark red metallic sheen while Enterobactor aerogenes develops into a bigger surface colonies with pale pink colour Non fermenters of lactose are colourless and do not affect the colour of the medium EMB agar contains methylene blue which inhibits gram- negative bacteria, while gramnegative lactose fermenters produce nucleated colonies (dark center). E.coli produces small colonies with green metallic sheen whereas E.aerogenes forms bigger colonies without metallic sheen. Materials 1. 2. Endo agar or EMB poured plates. Positive MPN tubes (gas production positive)

Procedure

Pour 15 -20 ml of melted Endo agar into sterile petriplate and allow to solidify. Take a loopful of the culture from the MPN tube and streak on the solidified hardened media. Incubate the plates at 37%C/24 hours.

Inference Presence of colonies showing dark red colour with metallic sheen of >0.5 mm diameter shows the presence of E.coli. BIS standard for portable water

9. MICROBIOLOGICAL ANALYSIS OF AIR Air is not a suitable natural environment for the growth and reproduction of micro-organisms but a few types of organisms (e.g. aerobic spore formers Bacillus, Sereina, Achromobacter, Micrococci and mold spores) may, however be found in association with dust particles suspended in the air. Air is also known as to be a medium for the transmission of infectious micro organisms (e.g. Bacteria and viruses). The air inside a bacteriological laboratory is frequently required to be sterilised by irradiation or fumigation using bactericidal chemicals (aerosols). Two methods are usually employed to assess the

Training Manual on Quality Assessment of Food Products

63

bacterial load of air inside a bacteriological laboratory. One is sedimentation method (exposure of culture plates) and the other is slit sampler method a known volume of air is directed on to a plate through a slit of 0.25 mm size, the plate is being mechanically rotated so that the organisms are evenly distributed over it. One cubic foot of air per minute is allowed to pass through the slit onto the culture plates and these samples of 1 10 cubic feet or more of air are tested for any colony forming units. Estimation of microbial counts in dairies helps to provide the number and types of micro-organism present in the atmosphere. Materials Sterile petriplates Sterile molten standard plate count agar Sterile molten Sabouraud agar Procedure

Pour plates with melted SPCA and sabouraud agar separately (15 20 ml) maintained at 450C - 500C. Allow the media to set. Remove the lids of the petriplates and expose wherever required (like laboratory, processing room, cold rooms etc.) for 15 minutes. After exposure, incubate the SPCA plates at 370C / 24 48 hours and sabouraud agar plates at 250C/ 3 - 4 days. At the end of incubation period, count the number of colonies in each plate and record. Prepare smears of typical bacterial colonies in each plate and examine for morphology by simple staining technique. Examine the mould colonies developed in sabouraud agar using the low power objective of a microscope. Record the observations.

Observation of the smears prepared from the Colonies

Inference In a well- ventilated room which is free from dust, microbial contamination of air (bacteria, yeasts and moulds) as determined by exposure of poured plates shall not exceed 20 colonies/ plate after a 15 minutes exposure.
64 Training Manual on Quality Assessment of Food Products

CHAPTER 3

Training Manual on Quality Assessment of Food Products

65

66

Training Manual on Quality Assessment of Food Products

QUALITY CONTROL OF MEAT


Dr.B.Karthikeyan
Assistant Professor, Collegeof food and dairy technology, Chennai - 52

Keeping Quality of Meat and Meat Products Fresh meat can be referred as a product, which has undergone imminent postmortem changes following slaughter but has not been subjected to any processing. However, fresh meat that has undergone freezing can be conveniently termed as raw meat. Some characteristics of fresh and raw meat need to be properly understood in order to achieve the best results in processing. Meat being a highly perishable commodity requires strict quality control right from slaughter operations till ultimate consumption. The basic objectives of quality control are: 1. 2. 3. 4. 5. Protection of public health Extension of product shelf life Provision of consumer satisfaction Compliance of regulatory legislation Competitive edge in the trade

The general principles of meat product quality control involve: 1. 2. 3. Raw material control Control of processing operations Finished product inspection and control

It is very difficult to examine meat and meat products for every pathogenic, toxigenic and spoilage microorganisms. However, a product cannot be improved unless some objective assessment of its quality cannot be improved unless some objective assessment of its quality is available. But the methods adopted should be simple with quick results. Hence, the following indicator organisms are relied upon to determine the sanitary and safety status of these items. Meat and meat products are extremely perishable, so special care and handling must be exercised during all operations. Deterioration begins soon after bleeding, as the result of microbial, chemical and physical process. These process were not curtailed they would soon make meat unfit for consumption. It is necessary to minimize deterioration in order to prolong the time during which an acceptable level of keeping quality is maintained. The absolute necessity of maintaining preventive controls during all handling and processing of meat, in order to optimise its acceptability and permits its shelf-life is obvious. A nuclear of methods are employed throughout the meat industry to retard deteriorate changes and extend the length of the keeping quality period. It depends upon the preservative method used and the inherit properties of the specific meat items in question.
Training Manual on Quality Assessment of Food Products 67

It is generally recognized that the post-mortem changes associated with the conversion of muscle to meat, and the subsequent storage and handling are accompanied by some deteriorate changes in respective of the precautions taken during processing and handling. The changes occur is dependent upon the prevailing handling processing and storage conditions hence, proper refrigeration for the control of microbial activity retards enzymatic activity as well as minimize the deteriorate effects and enhance the keeping quality of meat and meat products. The keeping quality characteristics of meat are depended upon the changes in pH, Water Holding Capacity (WHC), Extract Release Volume (ERV), Tyrosine Value (TV), Thiobarbituric Acid (TBA) Number, etc. VETERINARY ANTE MORTEM INSPECTION OF FOOD ANIMALS Objectives

To detect animals suffering from infectious diseases like anthrax and glanders which are communicable to man To detect diseases like tetanus and rabies which do not show any significant pathological changes on post mortem inspection To prevent the food poisoning outbreaks by preventing consumption of meat from animals slaughtered while sick To separate the obviously ill or with high temperature from healthy, those in advanced pregnancy or recently calved To mitigate and minimize acts of gross or unnecessary cruelty in the handling of livestock or those fatigued

Place

It should be carried out in lairage.

Time

Within 24 hours before slaughter, during the period of light

Instruments

Identification of tags, restraining equipments and thermometer

Decision of ante mortem examination


If the animal is normal and free from any symptoms of disease can be passed for slaughter Animals which are showing the symptoms of a disease or affected with a localized condition, such animals should be treated as suspect and their slaughter should be carried out in the isolation block after they completely recovered from the disease Young animals that lack normal muscular co ordination, animals in advanced pregnancy and recently calved and the animals which are showing the symptoms of infectious diseases should be categorized in to animals unfit for slaughter
Training Manual on Quality Assessment of Food Products

68

VETERINARY POST MORTEM INSPECTION Objectives


To detect and eliminate abnormalities including contamination It should be carried out as soon as possible after carcass dressing is completed It should be carried out with care in a hygienic manner and avoid un necessary cuts

Place of inspection

Slaughter hall

Equipment

Knives, saws, scissors etc.,

Inspector

Should be veterinarian with long clinical experience

Judgments The final judgment of the veterinary inspector is a result of total evidence produced by observation, palpation, smell, ante mortem signs and reports of laboratory tests. The main decisions or judgment are as follows

Approved for human consumption Totally condemned for human consumption Partially condemned for human consumption Conditionally approved for human consumption refers to treatment of meat under the supervision of meat inspector either by heat or cold treatment to make safe for human consumption. Inferior meat in certain region hygienic but lower standard meat is sold as inferior meat especially those countries where there is scarcity of protein. Approved for human consumption, with distribution restricted to limited areas: The meats from animals in an area under quarantine because of an out-break of contagious animal disease. In this case there must be no risk to public health and the meat must be restricted in sale to the affected area to avoid the possible spread of disease.

Differentiation of the organs of different species

Training Manual on Quality Assessment of Food Products

69

70

Training Manual on Quality Assessment of Food Products

Differentiation of meats of various species

Training Manual on Quality Assessment of Food Products

71

FRAUDULENT SUBSTITUTION OF MEAT AND ITS RECOGNITION Meats are generally sold in the form of small pieces or minced form. So the unscrupulous butchers will take it as advantage and indulge in the adulteration of meat. It is the duty of the meat inspector to detect this type of fraudulent practices. The most common adulteration practices that are adopted are

Beef for mutton Chevon for mutton Cat flesh for rabbit Horse flesh for beef Mutton for venision

It is necessary to assure the wholesomeness of meat to the public, which besides other measures, may necessitate the authentic identification of species of meats. The following methods can be used for meat identification. 1. Physical methods a. General appearance : color, consistency, odour

b. General characteristics of the body fat: color, consistency, quality etc.., 2. Anatomical methods a. Dentition

b. Bone percentage of carcasses c. Rib numbers and their degree of curvature

d. Characteristics of long bone. 3. Histological methods a. Muscle fibre length

b. Muscle fibre dia mt The diameter and number of muscle fibres determined by fibreoptic microscope, can also lead to specific identification. Dia mt of muscle fibres of buffalo is more than ox, whereas muscle fibres of buffalo are smaller than size and polygonal in cross section as compared tio large and irreugular muscle fibre sof ox. as far as other species are concerned, the size of muscle fibres decreases in the following order: pig, buffalo, sheep, goat, poultry. 4. Chemical methods a. Composition of meat

b. Myoglobin content
72 Training Manual on Quality Assessment of Food Products

c.

Glycogen content

d. Composition of body fat Glycogen content Horse flesh is richer in glycogen than the flesh of other animals. But the glycogen from the horse flesh commences to disappear from meat from the time of slaughter. Therefore examination for glycogen as to be made early. Liver of many animals particularly pig contains appreciable amount of glycogen so if the liver is used an ingredient there may be more glycogen. Composition of body fat Horse fat can be differentiated from lard, beef, mutton fat by its higher content of linoleic acid. Horse fat contains about 1-2% linoleic acid, other anuimal fats contain only about 0.1% of the linoleic acid Iodine value This test is based on the amount of iodine absorbed by the unsaturated fatty acids in the fat. The iodine value in horse fat is 71 to 86, beef fat -38 to 46, mutton fat 35 to 46 and in pork fat 50 to 70. Refractive index For horse fat it is 53.6, for beef fat not above 40 and for pig fat it is not above 51.9. Composition of fat Muscular fat content varies according to the meat species. The intra muscular fat in mutton is higher (13.3%) as compared to beef (2.6%), buffalo meat (0.9%), chevon (3.6%). Vitamin A is present in beef fat and mutton but absent in buffalo meat, chevon or pork. Myoglobin content Horse meat contains maximum myoglobin content(0.71%) much higher than the musculature of other animals. 5. Immunological / serological methods a. Precipitation test

b. Double immunodiffusion test c. Single radial immuno diffusion test

6. Electrophoretic methods a. Polyacrylamide disc electrophoresis

b. Polyacrylamide gel electrophoresis c. SDS PAGE

Training Manual on Quality Assessment of Food Products

73

7. 8.

Iso electric focusing ELISA

IDENTIFICATION OF SPECIES OF MEAT BY SEROLOGICAL TEST Objective: to identify the given meat sample Materials 1. 2. PBS,PH 7.2 Precipitation tubes

3. Standard antisera against meat of different species. Procedure of precipitation test: About 30 60 grams of meat sample to be tested is minced with 50 ml of sterilized phosphate buffer saline and kept at room temperature for 3 hrs or at 4C for 12 hrs (Before mincing the meat, the sample should be made fat free by washing with ether or chloroform). The minced meat is then filtered to obtain a clear filtrate. Then 0.1 ml of each of the standard antiseara raised against meat of different food animals is placed in a series of precipitation tubes to which 0.2 ml of meat without mixing up of the two solutions. In positive case a white ring filtrate is carefully layered over, is formed at the interface in 5 15 minutes. Results: record your results and interpret them. DETERMINATION OF PH OF MEAT Objective: To determine the pH of meat to know whether the meat sample is a good one or not. Materials 1. Digital pH meter 2. Distilled water 3. 4. Known pH buffer solutions Blender

Procedure Take 25 g portion of meat and homogenize it for 1 minute in a sterile blender at high speed with 100 ml of distilled water add just prior to blending. A portion of 50 ml of the above solution is used for pH determination by using digital pH meter. Put on the instrument 10 minutes before estimation starts, to warm up the instrument. Set zero by adjusting the sensitive knob. Place the electrode in known buffer solution of 4, 7 and 9.2 etc., separately and turn the pH range knob depending upon the range of pH. Adjust the correct pH by using set buffer knob. The temperature control is maintained at the approximate temperature of the solutions being tested. Remove the electrodes and wash blot the tip and place it in the meat slurry prepared. Turn the pH knob to 0 - 7 pH range. Read the pH of the solution directly on the scale. Remove the electrode, clean and blot it dry and place it in a beaker containing cotton and distilled water.
74 Training Manual on Quality Assessment of Food Products

BOILING TEST TO DETERMINE THE PRESENCE OF ABNORMAL ODOUR IN MEAT Objective: To determine the abnormal odour in the given meat sample. Materials 1. 2. Meat sample Pan

Procedure Cut a piece of meat about the size of the hand and rich in fat, 24 hours after slaughter. Keep the meat pieces in pan containing cold water. Bring it to boil and simmer with a lid on the pan. To test for the presence of an abnormal odour, lift the lid of the pan and smell the steam given off. When the meat is sufficiently cooked it should be removed from the water, incised and the cut surface should be smelt. Abnormal odours are often accompanied by an abnormal taste and if necessary, the meat and the water should be tasted. TEST FOR DURABILITY OR DECOMPOSITION OF MEAT Objective To determine the extent of decomposition in a given sample of meat. Materials 1. Meat sample free from blood, fat and connective tissue, obtained after 24 hrs of slaughter 2. Nitrazine yellow indicator (1 in 10000)

3. Porcelain dish Procedure The sample of meat to be tested should be taken in to a porcelain dish, over which the nitrazine yellow indicator solution should be poured. Wait for few minutes and observe the change in the colour of meat. Interpretation 1. 2. 3. Meat with a pH of 6.0 produces a yellow colouration and is classified as having good durability. Meat with a pH of 6.4 produces an olive green colouration is classified as having insufficient durability and is suspect. While meat with a pH of 6.8 shows a violet colouration is considered as of very low durability and is unfit for consumption. pH reading of over 6.5 is regarded as evidence that the flesh is of poor keeping quality.

Results: record your results and interpret them.


Training Manual on Quality Assessment of Food Products 75

TEST FOR DETERMINING PERFECT OR IMPERFECT BLEEDING Objective To determine the status of the carcass whether the animal was bled efficiently or not. Materials 1. 2. 3. 4. Meat sample Agglutination tube Malachite reagent Hydrogen peroxide

Procedure A meat extract should be prepared by adding 14 ml of distilled water to 6 g of meat sample. Allow the extract to stand for 15 minutes without disturbing it. Remove the sediments. The test is conducted by adding 0.7 ml of the extract to an agglutination tube, then add one drop of malachite reagent, mix it properly and add one drop of hydrogen peroxide. Shake the mixture until it is slightly foams and keep it aside for 20 minutes. If bleeding is satisfactory, the fluid is clear and of blue colour If a moderate degree of imperfect bleeding is present the fluid is cloudy and of a green colour. If there is marked degree of imperfect bleeding, the fluid is cloudy and of olive green in colour. Results record your results and interpret them. Determination of pH The pH is a measure of the acidity or alkalinity in solutions or water containing substances. pH values lower than 7 are considered acidic, while pH values higher than 7 are considered alkaline. A pH of 7 indicates neutrality. pH values are related to the concentration of hydrogen ions (H+) in the substance. pH measurement is useful for:

Evaluation of meat quality for further processing, in particular the water binding capacity Control of ripening of raw fermented products, which is connected with drop in pH Control of acidity of ingredients such as brines, marinades etc

The pH can be measured by following methods 1. 2.


76

Digital pH meter Chemical indicator method (Nitrazine yellow)


Training Manual on Quality Assessment of Food Products

a. Digital pH meter Portable instruments are battery driven and have glass electrodes. The pH value in meat and meat products can be measured by direct contact between the sensitive diaphragm of the electrode and the meat tissue. Through the diaphragm differences in electrical load between the meat and electrolyte solution (e.g. Potassium chloride KCl) inside the glass electrode are measured and directly indicated as the pH-reading. In raw fresh meat, it is recommended to spray small amounts of distilled water onto the tissue at the point of measurement (prior to inserting the electrode), because the operation requires some fluidity in the sample and the glass electrode should be thoroughly wet. The amount of water necessary will not appreciably alter the pH. For accurate pH readings the pH-meter should be calibrated before use and adjusted to the temperature of the tissues to be measured. The electrode must be rinsed with distilled water after each measurement. Requirement- Digital pH meter, distilled water, beaker, electrolyte solution. Procedure 1. 2. Blend 15 gm meat with 30 ml distilled water at 27-300C. Note the pH with a glass electrode pH meter.

b. Nitrazine- Yellow Test This test determines the acidity of meat. Requirements: Nitrazine- Yellow indicator, glass rod, petri plate Procedure i. ii. Take a piece of meat free of blood, fat, and connective tissue in a petri dish. Add nitrazine yellow indicator (1:10000) sufficient to cover the meat piece

iii. Mix with stirring rod iv. Note the colour change with standard chart provided. Interpretation

DETERMINATION OF EXTRACT RELEASE VOLUME (ERV) The technique was first described in 1964, has been shown to be a value in determining incipient spoilage in meat as well as in predicting refrigerator shelf life.

Training Manual on Quality Assessment of Food Products

77

Principle The technique is based on the volume of aqueous extract released by homogenate of meat when allow to pass through the filter paper for a given period of time, by this meat of good organoleptic and microbial quality release large volume of extract, whereas meat of poor quality releases smaller volume or none. Requirements: Beaker, distilled water, Whatman No. 1 filter paper, pestle and mortal, graduated cylinder. Procedure a) Take 25 g meat sample in 100 ml distilled water b) Bend it with in pestle and mortal c) Filter through Whatman No. 1 filter paper, folded thrice so as to make eight sections.

d) Allow the homogenate to seep between the folds e) f) Collect the extract in 100 ml graduated cylinder for 15 min. Record extract release volume and interpret results

Interpretation

DETERMINATION OF MEAT SWELLING CAPACITY Principle This test determines the freshness of meat Swelling capacity of meat increases during spoilage due to protein degradation and penetration of more amounts of water in protein matrix. A method of measuring the water binding capacity of muscle proteins with low water holding forces known as meat swelling (SW). Requirements Distilled water, centrifuge, blender, graduated cylinder Procedure
78

Take 25 g of meat in 100 ml of distilled water Blend it for 2 min Centrifuge 35 ml of homogenate at 2000 rpm for 15 min Measure the volume of supernatant (S) Record the volume and denote it as S .
Training Manual on Quality Assessment of Food Products

Percent meat swelling can be determined as DYE REDUCTION TEST Principle This test estimates bacterial population in meat sample indirectly. Requirements Resazurin dye / tablet, filter paper strips, polythene bag, nutrient broth, swab, distilled water Procedure- A. a) Four Resazurin tablet dissolved in 100 ml of water sample. b) Filter paper strips are dipped in above solution and dried in dark and cool room. c) For testing, the strip is moistened and a drop of meat juice to be tested is placed on it for 1 minute

d) The strip is then placed in polythene bag and kept in dark room (22-230 C) e) Time taken for the blue colour to the paper to change to red is noted

Procedure- B. a) Soak the swab in nutrient broth b) Sample 1 cm2 area of meat c) Break the swab in 10 ml nutrient broth yeast extract medium

d) Collect the washings in a sterile glass beaker contaning 0.3 ml freshly prepared 0.05% aqueous Resazurin dye e) f) Incubate the beaker at 30oC in a dark room Note the time taken for the change in colour from violet/ blue to colorless

Interpretation

Training Manual on Quality Assessment of Food Products

79

ESTIMATION OF EGG QUALITIES


Dr. A. Sundaresan
Assistant Professor, College of food and dairy technology, Chennai-52

External Characteristics and Grading of Shell Eggs A normal chicken egg is ovate in shape. Wide variation in shape may lead to breakages during handling and transport. For easy transportation and merchandising of egg, they should possess normal external characteristics. If shape and size are abnormal, the eggs are liable to break. Similarly, thin shell and weak shell egg or shell less eggs are liable to break and are unfit for transportation. Moreover, eggs with thin shells loose their quality quickly. Shell colour and other external characteristics will determine the market acceptability. Clean eggs will be sold at premium price, than dirty eggs. The external characteristics of the egg will be assessed by the following methods: 1. 2. 3. 4. 5. 6. 7. Egg size/ weight Shape Shell colour & Texture Cleanliness Volume Specific gravity Surface area

1. Egg size or weight Each species of bird has its own standard egg weight. Similarly the egg weight vary between breed and age of the bird. Heavier birds produce heavier egg. A normal chicken egg weighs 55-60gm depending upon the breed and age. The chicken egg will be about 1/30th of the hens body weight. In case of ducks, the egg weight ranges from 65-70gm, depending upon the breed, which will weigh 1/ 25th of its body weight. Goose lay eggs weighing 130-200gm, depending upon the breed. Japanese quail eggs will weigh around 10gm, which will be about 1/15th of its adult body weight. When compared to body size, Japanese quail lay heavier egg than other species. Turkey egg will weigh 65-70g, and it is only about 1/60th of its body weight. In all species of birds, older birds lay heavier eggs than younger birds. Record the weight of egg provided to 0.1gm accuracy using triple beam balance. Some times the egg size will be extremely small or large as in the case of yolk less/ double yolked eggs which are difficult to transport because they will break during transit. They are sold in the farm itself. 2. Shape The usual egg shape is ovate. The shape of the egg plays a major role in packing and transport. The normal shape of an egg can be marred due to diseases like Ranikhet and Infectious Bronchitis. Too small or too large eggs are discarded in the farm itself. Egg shape is expressed as Shape index. Here the process is to measure the maximum length of the egg using a vernier caliper and also the average width of the egg measured in two places. It is measured to an accuracy of 1mm and the shape index is arrived at by using the formula.
80 Training Manual on Quality Assessment of Food Products

Shape Index =

Average width ____________________ Average length

X 100

A normal egg will have a shape index of 72 (Range 70-74). Egg which is spherical in shape will have a shape index of 75 and above; such of those eggs which are elongated/ elliptical will have lesser shape index of 70. These eggs which do not fall into the normal range of the shape index cannot be used for hatching. 3. Shell colour and texture It indicates smoothness and roughness of shell surface and also indicates shell quality. Shell colour is due to the presence of pigments. Ooporphyrin gives brownish colour to the egg shell, which is normally seen in eggs laid by the Asian, the English and the American Class of birds. The pigments Oocyan causes other blue colour in eggs laid by the Aracauna breed. 4. Cleanliness This is essential for consumer satisfaction and also to improve and maintain the keeping quality. A dirty egg may harbour harmful microbes which will spoil the egg and render it unfit for consumption. Eggs collected from deep litter will be more dirty than caged eggs, obviously due to dirty wet litter and delayed collection of eggs. 5. Volume Volume is also one of the indicators of egg size. Egg volume is directly proportional to the egg size. Since the specific gravity of egg is more than one, the volume of a fresh egg will always be less than the egg weight. However a small egg will have greater volume by weight ratio. The egg volume of different species will be around 90-95% of their fresh egg weight. To measure the volume of the egg, fill a measuring cylinder of 500 ml/ 1 litre capacity with a known quantity of water. After noting the lower meniscus of the water, gently slant the measuring cylinder and slide the egg carefully into the measuring cylinder and note the final reading of the water, the difference in value will give the volume of egg in cm3. 6. Specific gravity This gives an indication of the egg shell quality, as well as its freshness. Fresh eggs will have higher specific gravity than old and long stored eggs, because there will be a loss of moisture in the old eggs which inturn replaced by air. So the air cell will become bigger as the egg is stored for a longer time. Similarly, eggs having stronger shell will have higher specific gravity than thin shelled eggs. The measure of specific gravity can be made by several methods. (i) By measuring the egg weight and then weighing the egg in water, to find the weight loss in water. (ii) By dipping the eggs in a salt solution having several concentration of salt dissolved in it; having a specific gravity ranging from 1.0-1.1 with an interval of 0.02. A normal egg will have a specific gravity of 1.06. Any value less than this may indicate that the egg is old or the eggs are

Training Manual on Quality Assessment of Food Products

81

thin shelled; irrespective of other criteria, smaller eggs will have high specific gravity due to more uniform shell. (iii) By knowing the egg weight and volume. Specific gravity = Weight of the egg in gram ____________________________ Volume in cc

7. Surface area It is calculated by using the formula

Where, 12.6 is a constant. Surface area of an egg is directly proportional to egg size. The surface area will be more for elongated eggs than for spherical eggs. Candling and grading of table eggs Table eggs While grading an egg, the external quality factors like shell and structure, soundness of the shell and shell cleanliness are the factors to be considered. The normal egg is oval in shape and the shell surface is expected to be sound, smooth and free from thin spots, strong and clean. Exterior egg quality factors 1. Shell shape and texture a. PRACTICALLY NORMAL A shell that is approximately the usual shape and that is sound and free from thin spots. Ridge and rough areas that do not materially affect the shape and strength of the shell are permitted (AA or A quality). b. ABNORMAL A shell that may be somewhat unusual or seriously misshapen, faulty in soundness or strength and showing pronounced ridges and thin spots will be down graded. 2. Soundness of shell a. SOUND An egg whose shell is unbroken.
82 Training Manual on Quality Assessment of Food Products

b. CHECK OR CRACK An egg that has a broken shell or crack in the shell but with its shell membranes intact and the contents do not leak. Checks may range from a very fine hair like crack (blind or body check) that is discernable only by candling. Eggs with blind checks will not keep well nor can stand even moderate rough handling and so should be used immediately. c. SMASHED An egg whose shell is smashed or shattered. d. LEAKER An egg that has a crack with a break in the shell and shell membrane to the extent that the egg contents leak out. 3. Shell cleanliness a. CLEAN A shell that is free from foreign material and from stains. An egg may be considered clean if it has only very small specs of stains and dirt. b. MODERATELY STAINED A shell which is free from prominent stain and adhering dirt, but which has moderate stains. c. DIRTY A shell which is stained prominently beyond 1/4th of its total surface area. A dirty egg will be downgraded. d. ADHERED DIRT Shell which have foreign dirty material stuck on it like faeces etc. This will be totally down graded or discarded. Candled out egg quality The interior quality of an egg without breaking it can be detected by candling the egg. For this we need a candler. The egg is held gently before the light that emanates from the candler and a gentle twist or twirl is given to the egg to observe the air cell and the yolk shadow. The air cell depth is measured using this candler and a cell depth gauge. The air cell is measured in mm at the broad end of the egg. 1. Air cell a. PRACTICALLY REGULAR In this, the air cell maintains a fixed position seen at the broad end of the egg. The outline of the air cell is clear in a white shelled egg.
Training Manual on Quality Assessment of Food Products 83

Aircell depth A fresh egg will have an air cell depth of less than 3mm (0.3cm). As the egg ages, the depth of the air cell increases. Aircell depth for different USDA Grades USDA Grade AA A B C b. FREE AIR CELL An air cell which moves freely between the intact membranes towards the uppermost point of the egg. This will downgrade the egg. c. BUBBLY AIR CELL A ruptured air cell inner shell membrane resulting in one or more small separate air bubbles usually floating in the albumen (B quality). 2. Yolk The yolk outline from egg candling is defined as: a. OUTLINE INDISTINCT OR SLIGHTLY DEFINED The yolk outline is indistinctly visible and appear to blend with the surrounding white as the fresh egg is twirled (AA grading). b. OUTLINE FAIRLY WELL DEFINED The yolk outline is visible but not clearly out lined as the egg is twirled (A quality). c. OUTLINE PLAINLY VISIBLE The yolk outline is clearly visible as a dark shadow when the egg is twirled (B quality). d. The yolk size and shape determined by grading egg candling is defined as (i) enlarged and flattened - A yolk in which the yolk membranes and tissue have weakened and/ or moisture has been absorbed from the white to such an extent that the yolk appear definitely enlarged and flat (B quality). Maximum depth 0.3cm (1/8th inch) 0.5cm (3/16th inch) 0.8cm (3/8th inch or less) Over 0.8cm (3/8th inch)

84

Training Manual on Quality Assessment of Food Products

The term used to describe yolk defects are a. PRACTICALLY FREE FROM DEFECTS The yolk shows no blastoderm development but may show other very slight defects on its surface (AA and A quality). b. SERIOUS DEFECTS The yolk may show well developed germ spots and other serious defects (B quality). c. CLEARLY VISIBLE GERM DEVELOPMENT Development of the blastoderm in the yolk that has progressed to the point where it is plainly visible, as a circular spot on the yolk with no blood (B quality). d. BLOOD DUE TO GERM DEVELOPMENT Blood carried by development of the blastoderm in a fertile egg to a point where it is visible as a definite line or a blood ring. These eggs are discarded. 3. Albumen The condition of the albumen is determined by candling as follows: a. CLEAR The albumen is free from discolouration of foreign bodies floating in it. Prominent chalazae should not be confused with meat spots (AA quality). b. THICKNESS Fresh egg will have a firm thick albumen which keep the yolk in central position. As egg becomes old, the albumen will become thin and watery and the yolk will be freely moving. c. MEAT SPOTS AND BLOOD SPOTS May be on the surface of the yolk or floating; it is greater than 0.3cm (1/8 inch) diameter (B quality) or if it is greater than 0.3cm (1/8th) diameter, the egg is discarded. d. BLOODY WHITE Blood has diffused through the white. This egg cannot be consumed hence discarded. Table 14.2: Ag-Mark (Agricultural Marketing act - 1937) weight specification for different Ag-mark Grade gm.

Training Manual on Quality Assessment of Food Products

85

Table 14.3: Label colour for different Ag-mark grades

Table 14.4: Bureau of Indian Standards (ISI grades) specifications for eggs

MEASURES OF INTERNAL EGG QUALITY The quality of egg can be best ascertained by breaking open the egg and studying the various parameters of the shell, albumen, yolk and also by objective evaluation. The equipment required are: 1. 2. 3. 4. 5. 6. 7. 8. Egg Egg breaking stand Vernier calipers Tripod stand Micrometer or Spherometer Screw gauge or shell thickness gauge Empty beakers Balance, kitchen knife, scoop etc. Roche yolk colour fan

The measurements to be taken are 1. 2.


86

Shell per cent Shell thickness


Training Manual on Quality Assessment of Food Products

3. 4. 5. 6.

Albumen index Yolk index Yolk colour Other abnormalities like blood spots, meat spots, germ spots and any other foreign bodies like worms etc.

1. Shell per cent This constitutes about 11-12% of the egg. The shell is dried with the membranes intact in a hot air oven at 105 5oC overnight, cooled and weighed. The result is expressed as per cent of total egg weight. Smaller egg will have a greater per cent than larger ones. 2. Shell thickness After breaking the shell, cut the membranes and peel. Take three pieces of shell, each piece is taken from three representative areas, namely from the narrow and broad ends and third piece at the equatorial region. A good quality chicken egg will have a thickness of 0.33mm, Japanese quail egg 0.13mm, Turkey egg 0.4mm and duck egg 0.3mm. 3. Albumen index The firmness of the egg white is correlated with the albumen quality. After breaking open the egg the height of the thick albumen is measured using a tripod stand micrometer or a spherometer, while the width and the diameter of the thick albumen is measured by using the vernier caliper. The height of the albumen increases in a fresh egg and slowly lowers as the egg ages. A fresh egg will have an albumen index of 0.1. The proportion of the thick and thin albumen can also be measured in percentage on total weight of the egg. A good quality egg will have 55% thick and 45% thin albumen. A sieve of 1/16th inch size is made use of to separate the thick and thin albumen. The quality can also be evaluated objectively using the USDA score chart or otherwise known as Van Wagenan chart, this has 12 pictures of break open eggs ranging from high, medium to low, each ranging from AA to C grades. Height of albumen in (mm) _______________________________ Average width of albumen in (mm)

Albumen index

4. Yolk index This is an expression of the spherical nature of the yolk. The height of the yolk is measured by micrometer and diameter is measured by using vernier calipers. The yolk index is a measure of the standing-up quality of the yolk. Height of yolk in mm = ____________________________ Average diameter of yolk in mm

Yolk index

Training Manual on Quality Assessment of Food Products

87

The average value for a fresh egg is 0.40 and above. As the egg becomes aged, it get flattened and the yolk index is lowered. 5. Yolk colour Even though the yolk colour is not an indication of its absolute quality, it may some times indicate the development of objectionable colours due to chemicals or microbial growth. The normal yolk colour is yellow to orange. Diets which are rich in carotenoid pigments especially Xanthophill, Cryptoxanthine, Leutein will impart dark yellowish/ orange colour in the egg-yolk. Birds fed with diets rich in yellow maize, alfalfa meal, groundnut leaf meal will have a deep orange colour yolk. A rich yolk colour is preferred by consumers. Olive green discolouration is objectionable. This is due to feeding layers with cotton seed oil cake. Sometimes there could be germ development, which is an indication of a fertilized egg. The colour of yolk is measured by various colour charts, colour disc, serially diluting solution of potassium-di-chromate or by using the Roche yolk colour fan. 6. Other abnormalities Many albumen and yolk defects like blood spots, meat spots, germ development, mottled yolks are noticed which may be due to infection, metabolic or nutritional defects. I. ALBUMEN DEFECTS 1. 2. WATERY ALBUMIN: This is seen in diseases like IB, ND (RD) or due to hormonal imbalance. VERMINOUS EGGS: Usually a worm may migrate through the cloaca into the upper portion of the oviduct and be enclosed in the egg. ADDLED EGG: Here yolk and albumen are mixed together, due to rupture of the vitelline membrane.

3.

II. YOLK DEFECTS a. DOUBLE BLASTODISC/ BLASTODERM b. YOLK MOTTLING Results from a known uniform distribution of water due to separation of the vitelline membrane, water and the chalaziferous layer of the albumen. Nicarbazine, a coccidiostat will cause yolk mottling. c. BLOOD SPOTS This is very common in egg and this could be due to internal haemorrhage, genetic factors and due to lower levels of Vitamin A and K. d. MEAT SPOTS These are degenerated blood spots that appear as meat spots in an egg and most of these are from sources other than blood or tissue debris.

88

Training Manual on Quality Assessment of Food Products

e. GERM DEVELOPMENT Normally seen in fertilized egg. Due to this a blood ring will be seen on the yolk. f. YOLK DISCOLOURATION Olive brown mottled yolks are produced due to excessive amounts of gossypol, found in cotton seed oil cake. It reacts with iron in the yolk to give a mottled appearance. Cotton seed also contains cyclopropenoid fatty acids which produce a pinkish discolouration of the albumen. g. YOLKLESS EGG These eggs are usually small in size, without the yolk and contain tissue debris or worm, in the place of yolk. Stepwise procedure for measuring internal qualities 1. 2. 3. 4. 5. 6. 7. 8. 9. Record the egg number and egg weight (gm). Candle the egg and record the air cell depth (mm). Break open the egg gently over the glass plate and record albumen and yolk height and width as in the Table 1 (do not disturb the egg contents). Record the shell weight separately. Remove the shell membrane and measure the shell thickness measured at 3 places. Broad, narrow and equatorial region. Record the defects if any such as blood and meat spots. Now transfer the yolk into a pre-weighed petridish and record its weight by difference, after removing excess albumen by rolling on a filter paper. Find out the weight of albumen by difference. Record the HU using HU micrometer or spherometer. Calculate the albumen index, yolk index and H.U. using the formula.

10. Record the yolk colour using Roche yolk colour fan. 11. Give your comments about the egg quality. DIFFERENT METHODS OF PRESERVATION OF EGG Hen eggs: The egg must not have been preserved by any process and must be free from taint, the shell must be clean and free from stains, sound of normal texture and shape. The contents must be free from blemish, the yolk central and translucent or faintly but not clearly outlined and freely mobile the white must be translucent and, clear and the air space must not exceed three-eighth of an inch in depth. Duck eggs: The eggs must not have been preserved by any process. The shell must be clean and free from stains, and sound the yolk central visible but not dense and freely mobile. The white must be translucent, firm and not watery.

Training Manual on Quality Assessment of Food Products

89

When an egg with these specifications is broken in a plate, the yolk stands up and the does not spread out. A flat yolk and a watery or spreading white indicate that the egg is not very fresh. A. preservation of Eggs In order to preserve eggs only good quality eggs should be produced. Therefore any method of preservation starts from the point of production itself. The following practices are recommended as routine for the production of quality eggs on the farm. 1. 2. 3. 4. 5. Collection of eggs at least 3 times daily. Using a clean receptacle with ventilated sides and bottom, preferably filler flats. Careful handling of eggs during collection and white storing in filler flats etc. Cooling the eggs quickly to 500F or less at 75-85% relative humidity. Marketing the eggs at least twice weekly.
PRESERVATION:

The shell of an egg normally carries a wide range of microorganisms on its surface which are mostly responsible for spoilage of eggs. Many methods have been used in the past to counteract this and extend the shelf life of eggs. These include: I. DRY PACKING Eggs are kept in an earthen pot with clean dry packing material and the pot is buried in wet sand. II. IMMERSION IN LIQUIDS This is fairly an old method and it primarily prevents the evaporation of moisture from the egg. Depending on the liquid used it may also inhibit bacterial decomposition by chemicals action or by physical means such as occlusion of air passages/ pores. 1. LIME WATER TREATMENT Limewater is prepared by mixing about 0.5kg of quick lime (calcium oxide) in about 1 liter of boiling water. The mixture is left to settle overnight and the clean supernatant liquid is poured out into a jar. Sodium chloride of 112 grams per liter may also be added to increase the specific gravity of water and will minimize then chance of breakage of eggs. In this solution, 2.5 liters of cold water is added and filtered through muslin cloth. Keep the eggs to be preserved in a glass jar or earthen pot and pour the lime solution over the eggs till all the eggs are completely immersed. Eggs have to be kept in this solution for 24 hours to get maximum beneficial effect. After 24 hours they are taken out, dried and arranged in filler flats. Eggs can be kept for 2-3 months in a good edible condition at normal ambient temperature. The only disadvantage however, is the taste of lime can be detected in the eggs.
90 Training Manual on Quality Assessment of Food Products

2. WATER GLASS METHOD A 10% solution of sodium silicate is prepared in hot water and allowed to cool. The cooled solution is poured into a jar containing the eggs till they are immersed completely. The jar is covered and kept in a cool place where the temperature should not exceed above 700F. Eggs preserved by this method are usually punctured before boiling to avoid the breakage of shell and it also helps for easy peeling of shell. For treating the eggs in limewater or water-glass proceed as follows 1. Take a clean, glazed earthen vessel or glass jar and place the egg in it in rows one above the other with their narrow ends down. Avoid too many layers in one vessel to prevent the breakage the lower due to an excessive weight above. Prepare water-glass solution or limewater in a separate vessel. Pour gently the water glass solution or lime water in the jar containing the eggs. Keep the level of the liquid 5 to 7 cm. above the uppermost layer of eggs. About 15 dozen eggs can be preserved in liters of the solution. Spread a thin layer of some oil over the water- glass solution to prevent the evaporation of water. The loss of water from the solution may increase its viscosity to an extent as to make the handling of eggs difficult. Cover the jars tightly and keep them is a cool place. The heat treatment of eggs for defertilisation and thermo-stabilisation before their preservation in the limewater or water glass solution will increase their keeping quality. You can keep eggs. So treated and preserved, for 10 to 14 days is summer and about four weeks, In winter, without refrigeration. For keeping a small number of eggs for home u8se, you can conveniently preserve them in the limewater or water glass solution the same way.

2. 3.

4.

5.

III. SHELL - SEALING TREATMENTS When the shell is sealed through this treatment then water vapour and CO2 do not escape and microorganisms are unable to penetrate the shell. COATING WITH OIL This is a fairly successful method of rendering the egg less permeable. It can be done by simply dipping the egg in a bowl of tasteless, odorless, colourless edible oil, Having a specific gravity of about 0.855 to 0.870 at 150C; viscosity should but be more then 70 to 90 and having a high pouring point so that so that at lower temperature it remains in the liquid form. The eggs are immersed only for a moment and are then removed and the excess oil is allowed to drain. If oil treatment is to be effective it should be done preferably at the point of production the day after the egg is laid. Oiling is not a substitute for refrigeration. These eggs must be held at a low temperature. Cotton seed, linseed and groundnut oil are good sealing agents but mineral oils are preferable since they are less subject to oxidative changes during storage. The rate of CO2 escape is considerably reduced in oil-immersed eggs and these eggs are not likely to absorb foreign odours. The oil treatment can be also be done by a hand or electric sprayer.
Training Manual on Quality Assessment of Food Products 91

Eggs can be sealed under vacuum. Oil may be successfully used in vacuum impregnation method. The egg is first immersed in oil and then subjected to reduced atmospheric pressure, when normal pressure is restored the tendency of the air to enter the pores of the shell causes the solution also to be drawn in. The oil does not penetrate through the egg membranes. The commercial egg treatments with oils are, 1. 2. 3. 4. 5. 6. 7. 8. 9. Heavy paraffin oil (Central Food technology Research Institute) Myvacet 9-40 (developed at CFTRI - Mysore) Myvacet 5 Myvacet 7 Petroleum jelly Liquid paraffin Paraffin wax Coconut oil Dalda

10. Carboxyl methyl cellulose 11. Technical white oil. 3. THERMOSTABILIZATION This method is good for fertile eggs since it kills the embryos and therefore is also known as defertilization method. It essentially consists of immersing shell eggs in hot water at 1300F for 30 minutes which tend to coagulate the albumin and then the egg is cooled under tap water. Treated eggs remain edible for 3 to 4 weeks even during summer months. Though this method has many advantages such as stabilizing of the albumin and sterilization of the egg shell, the egg looses the property of foaming to a remarkable extent. Embryonic development in fertile eggs is completely arrested. For carrying out the above treatment, proceed as follows: 1. 2. Take clean fresh eggs or high quality and put them in a wire basket. Heat clean fresh water (drinking) in a wide-mouthed vessel to 54.50C (1300F) Dip the wire basket contai9ning eggs in hot water for 15 to 30 minutes. Continue heating and keep in stirring constantly with a stirrer to maintain the temperature uniformly around all the eggs. Take the basket out of water and dry the eggs by spreading them in front of a fan.

4.

Advantages 1. 2. It was kill the surface bacteria. The therrnostabillisation also reduces the loss of moisture and the consequent drop in weight of eggs during storage..

92

Training Manual on Quality Assessment of Food Products

3.

It pasteurizes the eggs against most of the bacteria that cause spoilage during storage. It has been observed that themrmo-stabilished eggs remain edible for about 14 days during summer months. When kept at a room temperature of about 34C (93.2 F). The untreated eggs become inedible in about two days under such conditions. OVER WARPPING For over wrapping of eggs polyethylence, cellophane, polyvinylidence and other transparent, thin but sufficiently strong, films are used. Theses films should be impervious to gases and moisture. Over warping of eggs in different atmosphere like carbon dioxide, vacuum etc. have been tried.

4.

5.

COLD STORAGE This is the best and most efficient method for commercial storage. Eggs for cold storage must be clean, unbroken, free from fungus and other infections. A temperature of O. C or 30-32. F and relative humidity of 85-90% is recommended for cold storage of eggs to preserve them for 5 to 8 months. for short period of preservation of 2 to e months, eggs can be stored at 10-12C or 50-55C with a relative humidity of 60-70$ Intact eggs are held at the lowest possible temperature that will avoid freezing and bursting of the shells. It has been observed that intact eggs do not freeze at temperature between -1.5C and @C .The relative humidity must not go beyond 90%.

6.

DRIED AND FROZEN EGGS This is another method of preserving egg contents or edible eggs. Egg products for commercial utility are prepared by drying or freezing eggs. Albumin flakes, yolk and egg White powder can be produced by drying process. Frozen yolk or frozen egg white can be produced by freezing . For egg white power production the best known method is spray drying and for albumin flakes, pan or cabinet drying method is mostly adopted.

Indigenous methods of gee preservation In places where refrigeration facilities are not available, eggs may be kept cool for short periods by any of these methods: 1. If you have only a small number of eggs to store keep them either in an earthen pot or in a wire basket. Keep the container on a stand in a shaded place or an airy room, and cover it with a wet cloth, Keep the cloth always wet. Place eggs in a cabinet having wire- mesh on all its sides. Place a wafer tray on the top of the cabinet. Hang wet cloth curtains on all the sides of the cabinet. see that about half a meter of upper portion on the curtain is dipped in water in the tray. For storing a large s number of eggs, keep them in a room. which is cooled by hanging cloth on the doors, windows and by working a fan inside. Keep tiles always wet by constantly sprinkling water over them. In these methods, the temperature around the eggs is lowered by about 3-6C due to the evaporation of water from wet cloth curtain. But the effectiveness of these methods cooling egg is rather limited. It not advisable to store eggs for more than two or three days under such conditions. These methods are good during the hot dry weather only. For sufficient evaporation of water will take place on the wet curtains and keep the environment cool. during the hot humid weather keep eggs in an airy place where it is relatively cool.

2.

3.

4.

Training Manual on Quality Assessment of Food Products

93

QUALITY CONTROL OF FISH


S.Suriyapriya
Junior Research Fellow and Dr.A.Surendraraj, Assistant Professor, College of Food and Dairy Technology, TANUVAS, Koduvalli, Chennai- 600 052.

1. METHODS OF EVALUATING FISH FRESHNESS AND QUALITY FOR FISH Fish quality is usually evaluated by the common sensory methods using human senses. Chemical and physical methods are indirect procedures to determine the quality of fish and fishery products. Bacteriological quality is of paramount important in the fish evaluation of fish quality. Quality assessment by sensory methods Sensory analysis of food relies upon evaluation through the use of our senses. Sensory assessment is used throughout the fish industry to judge quality by sight, touch, odour and flavor. The appearance, odour, flavor, texture etc. are called the sensory characteristics of the food. Sensory methods are better at recognizing complexities and are more discriminatory than instruments. For sorting species and size, we use sight and touch. All visible signs of deterioration and loss of freshness are detected efficiently and rapidly by sight. For detecting defective fillets containing skin, bones or parasites in fish or flesh testing with fingers and eyes is the only effective method. Textural assessment For assessment of fish texture, there is no better substitute for sensory methods. Odour and Flavour Odour and flavor can be very effectively assessed by sensory means using the mouth and the nose. With some practice, the pattern of changes in odour between very fresh and very spoiled food can be differentiated easily and quickly by sensory means and the degree of freshness can be accurately determined. Similarly off odour due to cold storage and rancidity, taints and unusual odours are readily detected and their intensity judged reproducibly. Taste assessment is one of the satisfactory methods for quality assurance. The degree of sweetness or bitterness can be determined by tasting. Seven quality factors are the most important and reliable in the organoleptic examination of fish. 1) General appearance 2) Appearance of the fish 3) Texture of the raw fish 4) Odour of raw fish 5) Odour of the cooked fish 6) Flavor of the cooked fish 7) Texture of the cooked fish Application of sensory analysis includes quality control of raw materials and finished products, storage tests, development of new products, taints and off flavours, aroma research, consumer tests and hedonic tests.
94 Training Manual on Quality Assessment of Food Products

Types of sensory assessment There are two kinds of assessment generally followed (a) organoleptic testing (subjective method), (b) sensory testing (objective method). Subjective method is based in judgments and personal opinion is allowed a free rein. These methods are typified by the consumer trial in which a group of ordinary public numbering at least 20 to 50 is asked their views about or preference for some sensory aspect of the product. In objective assessment trained judges or assessors who concentrate on a well-defined attribute of the product are employed. Biases are minimized here. Subjective assessment The preference of consumer for frozen fish was examined in order to define changes in quality at different temperature of storage. A 9-point hedonic scale defined quality. The test procedure (by Torry Research Station) has proved useful in comparing or screening samples. In characteristics of frozen fish were distinguished. In U.K, the white fish authorities have been conducting consumer tests on fish products based largely on this method (measuring plate waste). Subjective sensory tests of eating quality are undoubtedly superior because they come closest to assessing the consumer responses. However, this is expensive. Objective Assessment It is dispassionate, unbiased and descriptive assessment of individual or group of quality factors. Trained tasters can easily differentiate between the changes in quality of fish during early stages of spoilage. Under this, four methods have been widely used for fish. I. Paired comparison

II. Ranking III. Triangle test IV. Scoring of attributes fresh fish sample I. Paired comparison This method is used to compare toughness frozen fish with fresh sample. II. Ranking Ranking is usually used to detect oil taints in fish and shellfish. III. Triangle test This test is often used in quality control to ensure that samples from different production batches are the same. Each panelist is presented with three samples, two of the same and one different. The panelist is asked to identify the odd sample. As far as possible, one sixth of the panel should be presented with each permutation to avoid bias. This method is popular, as it is easy to set up, requires fewer panelist and the panelist require little or no training. It is not useful for samples with a strong background flavor.

Training Manual on Quality Assessment of Food Products

95

IV. Scoring and grading for fish freshness Quantification of sensory data requires the use of a scale, where the person can assess the due to deterioration that occur smoothly and continuously through varying degree of intensity, i.e, a graded series of changes. In order to use the method in a consistent, scientific and meaningful way, attempts are made to put a number or a score against the changes that occur during storage under different conditions. Because different fish spoil at different rate and different markets have different requirement it is difficult to produce standard scoring system that covers all fish. Scoring is the most commonly used scientific method for assessing freshness of chilled fish. The determination in fish quality is followed with the aid of a set of score sheets covering each of the main aspects of quality such as appearance, odour, flavour and texture in a standard manner. Separate descriptive scales are used for each attribute and the range is 10 to 0. The scale of ten is absolutely fresh and zero is completely putrid; anything below four is unacceptable. The basic Torry scheme is commonly used in the UK fish industry to control the quality of wet fish both everyday trade and factory operations. Pooling of attributes made the scheme more useful for industrial purposes. Freshness grades Grades have the same measuring as scores; but simpler and less finely subdivided in the EEC schemes of grading fish four grades are given. In t his four grades (E, A, B and C) of freshness are laid down corresponding to the various stages of spoilage. E is the freshest and C is unfit for human consumption. The EC freshness grades are based on the sensory assessment of fresh fish using visual parameters of general appearance, texture, and physical properties of the skin and membranes and the odour of gills. The torry freshness grading scheme is given in the following table. Assessing freshness (Taste panel study) Preparation of sample Fish is to be tested must be steamed in a closed dish over boiling water for a time appropriate to the thickness of the pieces (20 minutes). The frozen sample should be thawed before steaming. The US method involves wrapping the sample in a single layer of aluminium foil and placing on a wire rack suspended over boiling water in a covered container. The packaged product should be steamed for 20 minutes. Scoring system for cod, haddock, whiting, coley and hake Fresh sweet flavor characteristic of the species Some loss of sweetness Slight sweetness and loss of the flavours Characteristic of the species Neutral flavor, definite loss of flavor but no off- flavours Absolutely no flavor as if chewing cotton wool Trace of off- flavours, some sourness but no bitterness
96

10 9 8 7 6 5

Training Manual on Quality Assessment of Food Products

Some off- flavours some bitterness Strong bitter flavours, rubber such as flavor,Slight sulphide such as flavor Strong bitterness, but not nauseating Strong off- flavours of sulphide, putrid, Tasted with difficulty environment.

4 3 1 0

Testing environment may influence the result. A special taste panel room is normally recommended. The environment shall have

An odour free room Proper lighting / coloured light Screened individual booths Preparation area close to the taste panel room Colour of the wall should be neutral Noise level minimum

Freshness grading system for whole chilled cod, haddock, whiting and red fish *

*Source: Cornell, J.J. (1995) Control of fish Quality

Training Manual on Quality Assessment of Food Products

97

Quality assessment by chemical methods In chemical assessment of quality, various compounds of spoilage in fish muscle are quantitatively determined and correlated with sensory characteristics. These compounds produced in fish muscle by autolytic enzymes, putrefactive microorganisms or by chemical reactions such as lipid oxidation. During spoilage, these compounds gradually accumulate in the fresh and hence their determination provides a measure of the progress of spoilage. The compounds found most useful as quality indices are: i) Volatile bases Basic, nitrogenous compounds such as ammonia, Trimethylamine oxide (TMAO), Trimethylamine (TMA) and Dimethyamine (DMA). Degradation products from Adenosine triphosphat (AIP) eg:- Inosine monophosphate, hypoxanthine Peroxides, hydroperoxides and aldehydes

ii) Nucleotides

iii) Lipid oxidation products Total Volatile Bases (TVB)

Total volatile bases refers to all the volatile basic compounds and comprises mainly Trimethylamine and ammonia. The TVB-N value along with TMA is the most common index of quality universally used for deciding the state of freshness of fish. Some TVB is present even in very fresh fish (<20 mg%). Spoilage bacteria produces volatile bases. A level of 35-45 mg TVB-N /100g of muscle is usually regarded as the limit of acceptability beyond which the fish can be regarded as too spoiled. Trimethylamine (TMA-N) Trimethylamine level in fish muscle is used as a more specific index of bacterial spoilage. The level of 10-15 mg TMA-N/100 g muscle is considered as the limit of acceptability. This level increases with storage time at ambient temperature in ice or in refrigerated seawater and hence forms a good index of food spoilage. Determination of TVB and TMA-N TVB and TMA-N can accurately be determined by Conway micro diffusion method. Conventional steam distillation method can also be adopted for the determination of both TVN and TMA. Here, the TCA extract of the muscle is made alkaline with NaOH in a steam distillation apparatus and the evolving bases are absorbed in 2% boric acid. The volatile bases are determined by titration with standard acid. Histamine as on index of spoilage In fish, including mackerel, tuna, bonito, herring and sardine the production if toxic amine (histamine) is an indication of spoilage. Histamine along with other amines (e.g. Cadaverine) causes high toxicity. Dark flushed fish have high histidine content and spoilage organisms convert it into histamines. USFDA restricts maximum level of histamine in fish tissue to 50 mg/100mg Histamine is determined either by the HPLC method or by spectroflurometric method.
98 Training Manual on Quality Assessment of Food Products

Indole as index of quality Indole production is an introduction of spoilage in shrimp. Indole is currently used by the USFDA to validate the sensory evaluation of shrimp decomposition. Shrimp with <25 mg/100 g indole is organoleptically acceptable. Indole is usually determined by spectroflurometric or spectrophotometric method of the AOAC. Nucleotide based method Chemical quality tests must accurately reflect the edibility or sensory quality of product. The nucleotide degradation products, especially, inosine monophosphate (IMP), hypoxanthine (Hx) or Kvalue clearly reflect the quality loss in fish. The presence of higher levels of IMP in the muscle indicates relatively high quality, whereas accumulation of inosine and hypoxanthine is an indication of poor quality. (i) Hypoxanthine, an index of quality Hypoxanthine content has been used for evaluating fish quality. The content increases with spoilage in many species of fish. Fish with Hx content of more than 2.5 umole/g is regarded as spoiled. Hypoxanthine content can be determined by the silver salt method or by enzymatic method. Recently , the enzyme immobilization technique and High Performance Liquid Chromatography (HPLC) method also used to measure Hx content in fish. (ii) K- Value K-Value has been defined as the ratio of inosine and hypoxanthine to total concentration of all other nucliotides, has been regarded as the most appropriate index of fish quality. K- value in fish muscle is determined by the excellent method of Ryder,1985 using HPLC. K- Value of fish is in the range of 20-25% and at rejection is usually above 50-60%. Rancidity Tests (i) Peroxide Value (PV) It measures peroxides and hypoperoxides. The most common method is based on iodometric titration, which measures the iodine produced from potassium iodide (KI) by the peroxide present in the oil. The PV is a good guide to quality of fat. Fresh oil should have PV 1 meq. On storage it may increase to 10 meq/kg. The oil from fish muscle is extracted into chloroform after dehydrating the muscle with anhydrous sodium sulphate. The solution is filtered. 10 ml of chloroform extract is taken in a conical flask and mixed with 3-5 ml of aldehyde free acetic acid. 1 ml of saturated KI solution added and the solution kept in the dark for 10 minutes. It is then titrated against standard (N/500) thiosulphate solution using starch indicator. PV= ml of N/500 thio / g of fat (ii) Thio-barbituric Acid value (TBA value) TBA measures the malonnaldehyde produced during fat oxidation. TBA reacts specifically with malonaldehyde to give a red chromogen, which can be determined spectrophotometrically. The test
Training Manual on Quality Assessment of Food Products 99

can be carried out in two ways, either directly in food, followed by steam distillation and allowing the distillate to react with TBA reagent or by preparing an extract of the muscle followed by colour development. The absorbance of the red coloured pigment is measured at 538 nm against a reagent blank. The TBA number is then calculated as milligram of malonaldehyde per kg sample, which is equal to 7.8 times the optical density (O.D). TBA number = O.D 7.8 The PV is measure of the first stage of oxidative rancidity and TBA the second. It can be said that if the PV is above 10-20 or TBA above 1-2 then the fish will, in all probability, smell and taste rancid. Instrumental method for assessing seafood quality (i) Freshness meter Based on the changes taking place in the electrical properties of fish muscle such as conductance and capacitance a freshness meter which has a scale reading from 1 to16 has been developed at torry research station (U.K) known as torry meter (FM). A similar meter with a wider range of 0-100 Intelectron known as Fish Tester (FT) has been developed in Germany. These meters give quick and reliable indication of fresh fish quality in tropical fish. In GR Torry meter, highest value of 16 is obtained for very fresh fish and the readings decrease with spoilage, however varies with species. The RT- freshness grader developed in Iceland is a commercial success in this series. The grade measurement is faster and correlates well with sensory (odour) and chemical (TMA- value) assessment of freshness. (ii) Texture measurement The texture of the fish is often a good measure of the quality and can be determined most often in a shear or compression cell. The Universal Testing Machine (UTM) and other commercial texturometers (RHEO TEXS, Japan) are used to measure objective textural quality. Microbial Methods Bacteria largely determine the quality of fresh and lightly preserved fish products. The amount of bacteria in foods serves as a general indicator of hygiene. Development of total bacterial count is widely used to assess the bacterial quality of fish. In freshly landed fish and shrimp, aerobic plate count (APC) will be in the range of 103 106 and when the levels rise above 107 organism/g, fish flesh begins to spoil visibly. Determination of total count Measurement of the total viable count (TVC) is the most common method for determination of bacteriological quality of sea food. The common pour plate method (in an agar media) is still most widely used for the determination of aerobic plate count. Direct count method using a microscope is a rapid way of estimating bacterial counts. Using phase contrast microscope the level of bacteria in a sample can directly be determined.

100

Training Manual on Quality Assessment of Food Products

Florescence microscope method has attained widespread acceptance. The method involves staining of cells using acridine orange and detection by Florescence microscopy. Using direct epifluorescence filter technique (DEFT), result can be obtained within 30 minutes. Determination of spoilage bacteria The action of spoilage organism on fish generates unpleasant odours and flavours. They produce hydrogen sulphide to trimethylamine and reduce trimethylamin oxide (TMAO). Shewanella putrifaciens is the most important fish spoilage bacteria of marine fish. Vibrionaceae are another important spoilage bacteria. They are determined by agar plate method using Peptone Iron Agar (which contains ferric citrate). The H2S producing bacteria are seen as block colonies due to precipitation of FeS. 2. CHEMICAL INDICES OF FISH SPOILAGE During spoilage of fish a number of biochemical reactions take place. By measuring the products of these biochemical reactions, the extent of spoilage can be measured. These products are classified into several groups namely bases, acids, sugars, lipids, nucleotides, proteins, enzymes and miscellaneous. Bases Ammonia Ammonia is formed when proteins are decomposed. Ammonia is formed only after putrifaction and hence, significant increase in ammonia content occurs only after spoilage. Total Volatile Nitrogen (TVN) Total Volatile Bases (TVB) As fish undergoes spoilage the content of TVN, TVB increases. TVN/TVB is used to determine early stages of spoilage. Trimethylamine (TMA) Trimethylamine oxide (TMAO) is present in fish especially marine fish. During spoilage TMAO is reduced to TMA. It is an index of spoilage, as the production of TMA is dependent upon the bacterial population. Histamine Scombroid fish contains plentiful amount of histidine. Spoilage bacteria act on histidine forming histamine. Histamine suggested as a possible index of spoilage. Acids Volatile acids (VA) Formic acid, acetic acid etc are formed during spoilage. Volatile acids are formed only after putrefaction. VA can be used as quality index. Individual acids are also used as quality indices.

Training Manual on Quality Assessment of Food Products

101

Sugars Glycolysis After death the glycogen present in the fish flesh is converted into lactic acid. There concentration of lactic acid determines the flesh pH ;lower lactic acid concentration results in higher flesh pH. Bacteria, which cause spoilage, are more active in flesh of higher pH. Lipids The deterioration of lipids has always been of primary concern to fishery technologists. Degradation of lipids falls into two categories: (i) Oxidation which leads to of odours and flavours. (ii) Hydrolysis which splits off free fatty acids. THIOBARBITRIC ACID (TBA) The TBA test has been reported to correlate with sensory measurements of oxidation rancidity. This test also gives a measure of oxidative rancidity. Carbonyls The oxidation of unsaturated fatty acids in the formation of carbonyl compounds whose assay is being considered as a rancidity index. Free Fatty Acids Prior to the appearance of oxidative rancidity in lean fish, there is a rise in lipid hydrolysis that leads to a build- up of FFA. Non essential (free) FA is more readily oxidized than are the esterified fats. FFA gives a measure of hydrolytic rancidity. Nucleotides Nucleotides undergo considerable changes during storage of fish ion ice and there is a rise in inosine and hypoxanthine. The breakdown of nucleotides seems to be an index of quality. Proteins Salt solubility Salt solubility of Protein decreases as the Protein denatures, Denaturation of Proteins may be due to cooking, freezing, frozen storage etc.
Cell fragility test

Protein denaturation can be evaluated by cell fragility test. It also gives us an ideal about the effectiveness of frozen storage.

102

Training Manual on Quality Assessment of Food Products

Electrical resistance As fish spoils the electrical resistance of tissue falls. Hence the measurement of electrical resistance can be used as a freshness test. a- aminonitrogen During spoilage tissue proteins are decomposed into peptides, amino acids, etc., thereby increasing the content of free-amino groups. Indole Indole is a degradation product of tryptophan, and its presence is an indication of advanced spoilage. Enzymes Aspartyaminotransferase During faulty freezing and frozen storage cell damage due to ice crystal formation occurs. Then aspartyaminotransferase enzyme is released into the thaw drip during thawing. Hence the content of this enzyme is a measure of extent of cell damage. Miscellaneous pH pH of fish tissue increases as the spoilage increases. Eye lens Opacity of the eye lens (enzymatic change) increases as the fish spoils.

Training Manual on Quality Assessment of Food Products

103

104

Training Manual on Quality Assessment of Food Products

CHAPTER 4

Training Manual on Quality Assessment of Food Products

105

106

Training Manual on Quality Assessment of Food Products

STORAGE GUIDELINES FRUITS AND VEGETABLES


Er.V.Perasiriyan
Assitant Professor, College of Food and Dairy Technology, Koduvalli, Chennai- 600 052.

Cold storage of fruits and vegetables was used extensively by our ancestors to keep food after the harvest season. In modern times, the year round availability of fresh produce in the supermarket has reduced the use of home storage. However, even today there are benefits of home storage, which make it a good alternative to buying produce from the store. Most importantly, home gardeners often have excess fruits and vegetables that cannot be consumed immediately but would store well. Even those without gardens can buy food in season when it is fresh and inexpensive and then store it at home until a later date. Both these options are cheaper than buying food in the winter when it is often quite expensive. In addition, stored food harvested at peak maturity from the garden usually has better flavor and a higher nutritional value. When harvesting your own produce for storage, or buying it locally in season, there are certain guidelines to follow which assure maximum quality and minimum spoilage of your stored food. 1. 2. 3. 4. 5. 6. Harvest fruits and vegetables at peak maturity or as near as possible. Only use produce that is free from all visible evidence of disease. Do not pick any fruit or vegetable that has severe insect damage. Handle food carefully after harvest so that it is not cut or bruised. Leave an inch or more of stem on most vegetables to reduce water loss and prevent infection. Use late-maturing varieties better suited to storage.

In general, use only the best food for storage. Damaged food is more likely to suffermold and bacterial decay during storage and thus should be used fresh, processed, or discarded. Once harvested, fruits and vegetables must be stored under proper conditions, the most important of which are temperature and humidity. Each fruit or vegetable has its own ideal set of conditions at which it will store most successfully for the maximum length of time. These conditions can be classified into four groups: 1. 2. 3. 4. Vegetables which require cold & moist conditions Vegetables which require cool & moist conditions Vegetables which require cold & dry conditions Vegetables which require warm & dry conditions

The tables on the following page list temperature and humidity requirements for most vegetables. In addition to proper temperature and humidity, all fruits and vegetables must be kept in a dark, aerated environment. While most vegetables like moist conditions, standing water must be avoided, as it will quickly lead to rot. Produce must not be allowed to freeze and should be protected from animal pests such as mice. It is important to remember that crops held in storage are still living plants, capable of respiration and affected by their environment. The goal of storage is to keep them in a dormant state. *One other note, fruits and vegetables should always be stored separately. Fruits release ethylene, which speeds the ripening process of vegetables. Fruits are also very susceptible to picking up the taste of nearby vegetables
Training Manual on Quality Assessment of Food Products 107

Table 1. Fruits & Vegetables that require cold, moist conditions

Table 2. Vegetables that require cool, moist conditions

108

Training Manual on Quality Assessment of Food Products

Table 3. Vegetables that require cool dry conditions.

Table 4. Vegetables that require warm dry conditions.

Indoor Storage There are many areas in dwellings that naturally provide, or can be adapted to provide, a variety of temperature and moisture conditions for storage. Assess your specific situation; if possible, use a thermometer to monitor temperatures in various areas of your building during the fall and winter to find locations that are convenient and most readily adaptable for food storage.

Any spot that is sufficiently and evenly cool (32-60 oF) can be adapted for some type of food storage. The relative humidity of these locations will also affect what can be stored there. Basements are generally the most logical place to adapt. Older homes are often less well-insulated, and have pantries, back halls, enclosed porches, sheds and bulkheads which are adaptable to storage. Homes heated with wood stoves often have a central area of radiant warmth and peripheral areas that are considerably cooler.

Training Manual on Quality Assessment of Food Products

109

Outdoor Storage In areas with cold winters, vegetables requiring cool to cold, moist conditions can be stored in any of several types of outdoor storage areas. Earthen storages, from simple mounds to more elaborate root cellars, naturally provide cool, moist, dark and even conditions for a fairly long time. All outdoor storages have the disadvantage of sometimes being inaccessible, as well as being subject to damage by rodents and other vermin. To be successful, any outdoor storage must have thorough drainage. A storage into which water settles will not keep produce and may result in total loss. Packing Materials Packing materials used in storage perform several functions- insulation against fluctuating temperatures, moisture retention, and reduction of disease transmission. In outdoor storages, clean straw, dry leaves, corn stalks, hay, or sawdust are commonly used for insulation. These materials may be readily available or can be purchased relatively cheaply from local farms or garden centers. A slightly more expensive alternative is peat moss. Use these materials for a single storage season only, as they can become contaminated with molds and bacteria. They often can be recycled as mulch in the garden. Moisture retention of produce is usually achieved with moistened sand, sawdust or peat moss. Plastic bags, lined boxes, crocks, metal cans with liners, or plastic garbage cans are all items that retain moisture. Perforate plastic bags or liners at regular intervals to allow air circulation and prevent condensation. Vegetables requiring moist storage should never be left directly exposed to air. Alternating layers of produce with packing materials reduces disease transmission. Wrapping individual items of produce with newspaper aids moisture etention and reduces the possibility of cross-transfer of odors and disease.

Timing of Storage Placing fruits and vegetables in storage, either in pits or in basement rooms, before cold weather starts in the fall is a frequent cause of early spoilage. One of the most difficult steps in successful storage is to keep the produce in prime condition from the time of optimum maturity until the night temperature is low enough to cool the storage area. The length of storage and retention of nutrients will be maximized if the produce can be stored under the proper conditions immediately after harvest.
110 Training Manual on Quality Assessment of Food Products

The following page contains a few examples of storage areas for fruits and vegetables. Refrigerator Storage One of the best ways to store small quantities of vegetables requiring cold or cool moist conditions is to use an old or extra refrigerator. The amount of current required to run a storage refrigerator is usually low because they are opened infrequently and can be located in an out of the way, cool location. For best storage, produce should be washed free of soil and placed into plastic bags with 2 to 4 holes for ventilation. The 5 or 10 pound bag size is usually most convenient for the average family. Vegetables in plastic bags do not wilt nearly so rapidly as those stored openly in the refrigerator. Outdoor Sheds Sheds, breezeways, enclosed porches, and garages can be used to store insulated containers. An insulated container stored in an unheated area should have 6-8" of insulation on the bottom, sides, and top, with 2-3" between layers of produce. Additional blankets or other coverings may be necessary depending on how cold the outside temperature reaches. Remember that produce must not be allowed to freeze! Basement Storage Room Modern basements with furnaces are generally at least 50-600F and dry. While this is appropriate for some types of food storage, in order to achieve the cool, moist conditions necessary for most fruit and vegetables it may be necessary to construct a separate room. This separate storage area should be located in the coldest part of the basement, away from the furnace. The north and the east sides of the house are preferred. Avoid heat ducts and hot water pipes that generate heat. The room should have an outside window for ventilation. While the exterior walls do not need to be insulated, the inside partitions should have 3 thick fiberglass insulation. Faced insulation should have the vapor barrier closest to the warm side of the storage. If unfaced insulation is used, a vapor barrier such as 6-mil thick polyethylene can be used. The ceiling also requires insulation and a vapor barrier. Temperature can be controlled in this storage room by opening and closing the outside window. Humidity can be kept high by pouring water on the floor or by keeping wet burlap sacks or some similar material in the room.

Training Manual on Quality Assessment of Food Products

111

ADULTERANTS IN FOODS AND ITS DETECTION METHODS


Dr.A.Karthiayani, Mrs.K.Sudha
Assistant Professors, College of Food and Dairy Technology, Koduvalli, Chenna-52

Adulterant means any material which is or could be employed for the purpose of adulteration. Adulterated- an article of food shall be deemed to be adulterated if any one or more of the following had happened (a) If the article sold by a vendor is not of the nature, substance or quality demanded by the purchaser and is to his prejudice, or is not of the nature, substance or quality which it purports or represented to be. (b) If the article contains any other substance which affects, or if the article is so processed as to affect, injuriously the nature, substance or quality thereof. (c) If any inferior or cheaper substance has been substituted wholly or in part for the article so as to affect injuriously the nature, substance or quality thereof. (d) If any constituent of the article has been wholly or in part abstracted so as to affectinjuriously the nature, substance or quality thereof (e) If the article had been prepared, packed or kept under insanitary conditions whereby it has become contaminated or injurious to health (f) If the article consists wholly or in part of any filthy, putrid, rotten, decomposed or diseased animal or vegetable substance or is insect-infested or is otherwise unfit for human consumption. Preservative means a substance when added to food, is capable of inhibiting, retarding or arresting the process of fermentation, acidification or other decomposition of food. Preservatives shall be classified into following classes :(i) Class I Preservatives: Addition of Class I preservatives in any food is not restricted unless otherwise provided in the rules. Examples are are Common salt, Sugar, Dextrose, Glucose, Spices, Vinegar or acetic acid ,Honey and edible vegetable oils (ii) Class II preservatives are Benzoic acid including salts thereof, Sulphurous acid including salts thereof, Nitrates or Nitrites of Sodium or Potassium in respect of food like ham, pickled meat, sorbic acid including its sodium, potassium and calcium Salts, propionates of calcium or sodium, lactic acid, acid calcium phosphate, Nisin , Benzoate, Propionic acid including esters or salts thereof, Sodium diacetate and Sodium, potassium and calcium salts of lactic acid.

112

Training Manual on Quality Assessment of Food Products

Quick Test for some Adulterants in Food

Training Manual on Quality Assessment of Food Products

113

114

Training Manual on Quality Assessment of Food Products

Training Manual on Quality Assessment of Food Products

115

116

Training Manual on Quality Assessment of Food Products

Training Manual on Quality Assessment of Food Products

117

118

Training Manual on Quality Assessment of Food Products

CHAPTER 5

Training Manual on Quality Assessment of Food Products

119

120

Training Manual on Quality Assessment of Food Products

QUALITY TESTING OF BAKERY PRODUCTS


Mathanghi.S.K
Assistant Professor, College of Food and Dairy Technology

The availability of accurate models to predict product quality is an essential requirement in quality driven food process design. With this perspective quality testing of raw materials and functional quality test were portrayed in this chapter. QUALITY TESTING OF FLOUR AND BAKERY PRODUCTS Flour quality may be defined as the ability of the flour to produce an attractive end product at competitive cost, under conditions imposed by the end product manufacturing unit. The tests most commonly used to predict the quality of wheat flour and bakery products are described as follows. MOISTURE CONTENT Apparatus 1. Wiley Laboratory Mill, intermediate model, equipped with 18 or 20-mesh screen or any other mill that will grind to same degree of fineness without under exposure to atmosphere and without appreciable heating. Oven (either gravity-convection or mechanical convection). Capable of being maintained at 130C (+1) and provided with good ventilation. Thermometer shall be so situated in oven that tip of bulb is level with top of moisture dishes but not directly over any dish. Moisture dishes having diameter of 55 mm. and height of 15 mm. They should be of heavygauge aluminum with slightly tapered sides and provided with tightly fitting slop in covers. Before using, dry for 1 hr. at 130C, cool in desiccator, and obtain tare weight. Airtight desiccator containing activated alumina. Balance, accurate to at least 1 mg.

2.

3.

4. 5.

Method 1. Grind a 30 to 40 g sample in mill, leaving minimum possible amount in mill. Mix rapidly with spoon or spatula and transfer immediately a 5g portion to tared moisture dishes. Cover and weigh dishes at once. Subtract tare weight. And record weight of sample. Dismantle and clean mill between samples. Uncover dishes and place them with covers beneath on shelf of oven. Insert shelf in oven at level of thermometer bulb. Heat for exactly 60 min. after oven recovers its temperature of 130C. Remove shelf and dishes from oven, cover rapidly (using rubber finger insulators), and transfer to desiccator as quickly as possible. Weigh dishes after they reach room temp. (45-60 min, usually). Determine loss in weight as moisture (see equation 1). Replicate determination must check within 0.2% moisture.
121

2.

3.

Training Manual on Quality Assessment of Food Products

Calculation (A - B) Moisture (%) = 100 (A - C) Where, A = wt. of flour + Aluminium dish before drying B = wt. of flour + Aluminium dish after drying C = wt. of aluminium dish Standard values in flour ISI 13.0% PFA 14.0% PROTEIN CONTENT Principle Protein in wheat flour and bakery products is generally measured using the Kjeldahl method. This method estimates the total nitrogen in a sample and assumes a constant relationship between total nitrogen and the protein in wheat. The results are expressed by multiplying the nitrogen content by 5.7 factor and hence this method is reported to measure crude protein. Method 1. 2. 3. Place 1g sample in digestion flask. Add 0.7g HgO or 0.65g metallic Hg, 15g powdered K2SO4 or anhydrous Na2SO4, and 25 ml H2SO4. Place flask in inclined position and heat gently until frothing ceases. If necessary, add small amount of paraffin to reduce frothing. Boil until solution becomes clear. Cool to 25C and add 200ml distilled water. Then add 25 ml of sulfide or thiosulfate solution and mix to precipitate Hg. Also add few Zn granules to avoid bumping, tilt flask and add NaOH without agitation. Immediately connect flask to distilling bulb on condenser and with tip of condenser immersed in standard acid and 5-7 drops indicator in receiver. Rotate flask to mix contents, then heat until all NH3 had distilled. Remove receiver, wash tip of condenser and titrate excess standard acid in distillate with standard NaOH solution. Correct for blank determination on reagent.

4.

5.

Calculation % Nitrogen (N) = [(ml standard acid normality acid) (ml standard NaOH normality NaOH)] 1.4007/g sample Multiple % N by 5.7 to get % protein.
122 Training Manual on Quality Assessment of Food Products

ASH CONTENT Principle Total ash is the inorganic residual remaining on incineration in a muffle furnace. This reflects the quantity of mineral matter present in the flour. Acid insoluble ash reflects added mineral matter in milled products such as dirt, sand, etc. General method Weigh 10 g of the sample into a weighed silica dish. Incinerate it over a burner or in the muffle. Keep the dish in a muffle furnace maintained at 550-600C until light grey ash results or to a constant weight, cool in a desiccator and weigh. Rapid method Reagent: Alcoholic Magnesium Acetate Solution Dissolve 15 g Magnesium Acetate Tetra Hydrate (Mg (C2H3O2) 4 H2O) in alcohol and make up to 1 litre. Determination Weight 10 g of flour into a weighed silica dish. Add 10 ml. of the reagent. Let the mixture stand for about 2 minutes. Evaporate the excess alcohol in a water bath and keep in muffle furnace maintained at 750C-850C for 30-45 minutes. Remove the dish, cool in a desiccator and weigh. Determine the blank on 10 ml of the solution. Deduct blank from ash. Acid insoluble Ash Boil ash obtained in method 1 with 25 ml HCl (1: 2.5) for 5 minutes on a water bath, covering the dish with watch glass. Filter through ashless filter paper (No. 40). Wash the residue with water until free of acid. Ignite at 600C for 20 min, cool and weigh. Calculation W3 - W1 Ash = 100 W2 - W1 Where, W1 = Wt. of silica dish W2 = Wt. of silica dish + sample W3 = Wt. of silica dish + ash W4 - W1 Acid insoluble ash (%) = 100 W2 - W1 Where, W4 = Wt. of silica dish + acid insoluble ash.
Training Manual on Quality Assessment of Food Products 123

PFA limits: On dry basis Ash (%) Acid insoluble ash (%) QUALITY OF FAT

Atta 2.00 0.15

Maida 1.00 0.10

Butter is distinguished from other fats by the presence of glyceryl esters of relatively low molecular weight fatty acids, especially butyric but also caproic, capric, caprylic, lauric and myristic acids. These acids are wholly or partially steam volatile and water soluble. The Reichert value reflects the amount of butyric and caproic acids present and Polenske chiefly capryilic, capric and lauric acidwith some contribution from myristic and even palmitic acid Determination of Reichert-Meissl and Polenske Value 1. The Reichert-Meissl value is the number of millilitres of 0.1N aqueous sodium hydroxide solution required to neutralise steam volatile water soluble fatty acids distilled from 5g of an oil/fat under the prescribed conditions. It is a measure of water soluble steam volatile fatty acids chiefly butyric and caproic acids present in oil or fat. The Polenske value is the number of mililiters of 0.1N aqueous alkali solution required to neutralise steam volatile water insoluble fatty acids distilled from 5g of the oil/fat under the prescribed conditions. It is a measure of the steam volatile and water insoluble fatty acids, chiefly caprylic, capric and lauric acids present in oil or fat.

2.

Apparatus a. An all-glass distillation assembly conforming to specifications given in Methods of Analysis, AOAC- 17th Edn.,2000 Figure 925.41, chapter 41 page 14.

b. 25 ml beaker c. 100 ml graduated cylinder

d. 100 ml pipette e. f. Graduated burette Asbestos board with a hole about 65 mm dia for supporting the flask over the burner. During distillation the flask shall fit snugly into the hole of the board to prevent the flame from impinging on the surface of the flask above the hole.

g. Bunsen burner sufficiently large to allow completion of distillation in the prescribed time. capric and lauric acid glycerides. These fatty acids are steam volatile but not soluble in water, and hence give high Polenske value. Reagents a). Glycerine: b). Concentrated sodium hydroxide solution: 50 % (w /w) Dissolve Sodium Hydroxide in equal wt of water and store solution in a bottle. Use clear solution free from deposit.
124 Training Manual on Quality Assessment of Food Products

c.) Pumice stone grains d.) Dilute sulfuric acid solution: Approximately 1.0 N e.) Sodium hydroxide solution: 0.1N solution in water, accurately standardised f.) Phenolpthalein indicator: Dissolve 0.1 g of phenolpthalein in 100 ml of ethyl alcohol g.) Ethyl alcohol: 90% by volume and neutral to phenolphthalein Procedure 1. Weigh accurately 5 0.1g of filtered oil or fat sample into a clean, dry, 300ml distilling flask. Add 20 ml of glycerine and 2 ml of concentrated sodium hydroxide solution, and heat with swirling over a flame until completely saponified, as shown by the mixture becoming perfectly clear. Cool the contents slightly and add 90 ml of boiling distilled water, which has been vigorously boiled for about 15 min. After thorough mixing the solution should remain clear. If the solution is not clear (indicating incomplete saponification) or is darker than light yellow (indicating over-heating), repeat the saponification with a fresh sample of the oil or fat. If the sample is old, the solution may sometimes be dark and not clear. Add about 0.6 - 0.7 gm of pumice stone grains, and 50 ml of dilute sulfuric acid solution. Immediately connect the flask to the distillation apparatus. Place the flask on asbestos board so that it fits snugly into the aperture. This will prevent the flame from impinging on the surface of the flask above the level of the liquid and avoid super heating. Heat very gently until the liberated fatty acids melt and separate. Then set the flame so that 110 ml of distillate shall be collected within 19 to 21 min. The beginning of the distillation is to be taken as the moment when the first drop of the distillate falls from the condenser in the receiving flask. Keep the water in the condenser flowing at a sufficient speed to maintain the temperature of the outgoing water from the condenser between 15 and 20C. Collect the distillate in a graduated flask. When the distillate exactly reaches the 110 ml mark on the flask, remove the flame and quickly replace the flask by a 25 ml measuring cylinder. Stopper the graduated flask and without mixing place d it in a water bath maintained at 15C for 10 min so that the 110 ml graduation mark is 1 cm below the water level in the bath. Swirl round the contents of the flask from time to time. Remove the graduated flask from the cold water bath, dry the outside and mix the content gently by inverting the flask 4 to 5 times without shaking. Filter the liquid through a dry, 9 cm Whatman No. 4 filter paper. Reject the first 2-3 ml of the filterate and collect the rest in a dry flask. The filtrate should be clear. Pipette 100 ml of the filtrate and add 5 drops of the phenolphthalein solution, and titrate against standard 0.1N sodium hydroxide solution. Run a Blank Test without the fat, but using the same quantities of the reagents.

2.

3.

4.

5.

6.

7.

Training Manual on Quality Assessment of Food Products

125

Calculation Reichert-Meissl Value = (A B) x N x 11 where, A = Volume in ml of standard sodium hydroxide solution required for the the test; B = Volume in ml in standard sodium hydroxide solution required for the blank; and N = Normality of standard sodium hydroxide solution. Determination of Polenske Value After titrating the soluble volatile acids, detach the still head and rinse the condenser with three successive 15 ml portions of cold distilled water passing each washing separately through the measuring cylinder, 110 ml graduated flask and the filter paper and allow all of it to pass through. Discard all the washings. Place the funnel on a clean conical flask. Dissolve the insoluble fatty acids by three similar washings of the condenser, the measuring cylinder, the 110 ml flask with stopper, and the filter paper with 15 ml portions of ethyl alcohol. Combine the alcoholic washings in a clean flask, add 5 drops of phenolphthalein indicator solution, and titrate with standard (0.1N) sodium hydroxide solution. Polenske value = 10 x V x N where,V = Volume in ml of standard sodium hydroxide solution required for the test; and N = Normality of the standard sodium hydroxide solution. DIASTATIC ACTIVITY AND MALTOSE VALUE Principle The diastatic activity is the test, which reveals the extent to which the diastatic enzyme alpha-and beta-amylases produce sugars while acting on starch present in the flour. Normally, wheats have sufficient beta-amylase activity but lack in alpha-amylase activity. However, amylase activity increased thousand folds during wet harvest or germination. The diastatic activity is expressed as mg maltose produced/10 g of flour in one hour at 30C. The optimum level is between 2.5 to 3.5 (150 to 350 mg/10.0 g flour). Reagents 1. 2. 3. 4. 1: 5 Sulphuric acid (200 ml concentrated sulphuric acid made unto 1 litre). 15% solution of sodium tungstate Fehlings Solution A: Weigh accurately 69.28 g of copper sulphate and make up the volume to 1 litre with distilled water and filter. Fehlings Solution B: Weigh accurately 346g of sodium potassium tartrate and 106g of sodium hydroxide pellets and make up the volume to 1 litre with distilled water. The solution is kept overnight and filtered through glass wood. Methylene blue: 1% solution in distilled water.
Training Manual on Quality Assessment of Food Products

5.
126

Method Place 15g of flour in a 250 ml dry bottle and add 15 ml of water at 27C. Keep the bottle with the contents at 27C for one hour, the contents of the bottle being mixed by shaking once every 15 minutes during this time. At the end of the digestion period, add 1.5 ml of 1: 5 H2SO4 (Reagent No. 1) and 3.5 ml of sodium tungstate (Reagent No. 2) to stop the reaction. Filter immediately through No 1 filter paper and the clear filtrate is used for the determination of sugar content. Take Fehlings solution A (5 ml) and Fehlings solution B (6 ml) in a 250ml conical flask. Place the flour extract in a 50ml burette. Heat the mixed Fehlings solution on a burner and run at least 15-20ml of flour extract into the flask. Add 5 drops of methylene blue, heat to boiling and continue boiling for one minute, then add additional extract slowly at a time while still boiling until the blue colour disappears. An extra drop of indicator is helpful at the end. Repeat the titration. Calculate the maltose value from the Table 1. The maltose figure of flour sample should preferably be between 1.5 and 2.3. Table.1. Maltose figures corresponding to various titration levels

STARCH DAMAGE CONTENT Principle Starch damage influences water absorption capacity and dough handling of flour. Damaged starch is readily susceptible to action by amylolytic enzymes as compared undamaged starch resulting in the formation of dextrin. Desired level of damaged starch in bread flour should be 7-9%. Higher damaged
Training Manual on Quality Assessment of Food Products 127

starch is not advisable. This method determines the percentage of starch granules in flour or starch preparations, which are susceptible to hydrolysis by alpha-amylase. Apparatus 1. 2. 3. 4. Constant temperature water bath regulated at 30 + 1C. Micro burette 10ml capacity Pyrex test tubes 25200mm Boiling water bath and holder for large test tube.

Reagents 1. 2. 3. 4. Acetate buffer: Dilute 4.g anhydrous sodium acetate and 3.0 ml glacial acetic acid to 1 liter with water and adjust pH to 4.6-4.8. Sulfuric acid solution: Add 100ml reagent grade concentrated sulfuric acid to approximately 700ml water; dilute to 1 liter. Final solution should be 3.68N + 0.05. Sodium tungstate solution: Dissolve 18.0g sodium tungstate in water and dilute to 100ml. Alpha-amylase solution: Dissolve a suitable fungal alpha-amylase preparation (containing 5000 SKB units/g) in reagent No. 1 in proportion of 1.0g enzyme preparation per 450ml buffer. Filter rapidly using three course filter paper. This solution should be used with in 2 hr.

Method 1. 2. Bring reagent 4 to 30C. Weigh 1.0g of flour into 100ml stopped conical flask and add 45 ml of reagent 4. Keep it in water bath at 30C for exactly 15 minutes. At the end of 15 minutes, add 3.0ml of reagent 2 and 2.0ml of reagent 3. Mix thoroughly, let it stand for 2 minutes and filter through whatman No. 4 filter paper, discarding first 8-10 drops of filtrate. Immediately pipette 5.0ml of filtrate into 25200mm Pyrex test tube having 10ml of pot ferric acids solution. Immerse test tubes into vigorously boiling water for 20 minutes. Cool test tubes contents under running tap water and pour at once into 100 or 125ml conical flask. Rinse the test tube with 25 ml of acetic acid salt solution. Add 1 ml of soluble starch-KI solution. Mix thoroughly and titrate with 0.IN sodium thiosulfate to complete disappearance of blue colour. Run a blank without sample.

3. 4.

Calculations 1. 2. Subtract mg maltose equivalent found from Blank-sample. Result of calculations multiplied by 0.092 equals % damaged starch. % Damaged starch = mg maltose equivalent (B-S) 0.082. from table. B = ml of thiosulphate used for Blank S = ml of thiosulphate used for sample.
128 Training Manual on Quality Assessment of Food Products

FLOUR COLOUR GRADE VALUE Principle The colour test on flour sample indicate the whiteness, which is considered as a quality attribute as it affects appearance of final product. The colour of the flour depends on extraction rate of flour, amount of pigments and flour particle size. The darkness or whiteness of the flour is due to contamination of bran particles. Higher the flour extractions rate, darker the colour of the flour and vice versa. The coarse flour generally looks dull and darker than its finer counter part due to the shadow effects of the larger particles. Kent-Jones and Martin flour colour grader measures the colour of the flour based on the principle of reflectance. Method Develop a flour paste and place the paste in a glass cell in the instrument. The paste will reflect light at a wavelength of 540nm. The light spectrum is filtered and measurement gives a single number the Flour Colour Grade (FCG). Low values of FCG correspond to white flour. The flour colour is influenced by variety, microbial contamination, grain conditioning prior to milling, grinding and sieving conditions. FLOUR PARTICLE SIZE DISTRIBUTION Principle Particle size distribution of flour indicates friability of wheat endosperm under conditions of milling. Hard wheat generally yields larger particle flour, whereas soft wheat generally gives flour with finer particles. Fisher Units (FU) represent particle size of flour. Stack of sieves is generally used to determine the particle size distribution of flour. Fisher Units (FU) is the average diameter as measured by Fisher Subsieve analyzer. Flour coarser than 22 FU will be granular, dark in colour and will have low water absorption capacity. Flours finer than 16 FU will look extremely white but will be difficult to move through pneumatic systems and may have higher than normal starch damage. The finer fraction have low protein content and give greater cookies spread that the coarser fractions. Stokes Effective Diameter (SED) referred to as the Sedimentation Method of particle size analysis is also used. CONCLUSION The raw material of foremost importance in bakery product is the wheat flour. Bakery units prefer the flour obtained by milling in roller flourmill with 70-72 percent extraction. The composition of flour must have the optimum proportion of its constituents like protein, lipids, enzymes, starch, etc for processing of flour into a suitable and acceptable product.

Training Manual on Quality Assessment of Food Products

129

PERMISSIBLE LIMIT OF CONTAMINANTS, TOXINS AND RESIDUES IN VARIOUS FOOD PRODUCTS


Er. G. Velayudham
Assistant Professor , Dr.D.Baskaran, PhD, Professor2, Dr.B.Suresh Subramanian,PhD, Professor3 College of Food and Dairy Technology, Chennai-52.
1

This article regards the gaining knowledge of the contaminants, toxins and residues used in the various food products and it induces a worst effect in the human body and leads to death. To avoid these type of adulteration in the food products the Government of India has make draft regulation on Food Safety and Standard Act 2011(contaminants, toxins and residues) for the consumer safety purposes. The various types of contaminants are restricted to use over the food products are metal contaminants, crop contaminants and residues. Metal contaminants Food products specified in the below column should not contain any metal particles in excess of the quantity mentioned.

130

Training Manual on Quality Assessment of Food Products

Training Manual on Quality Assessment of Food Products

131

Crop Contaminants The foods products have limit to some amount of crop and naturally occurring toxic substances, beyond that it causes as adulteration.

132

Training Manual on Quality Assessment of Food Products

Naturally occurring toxic substances The foods products should not have the natural toxin beyond the maximum limit.

Residues The any type of insecticides shall not be used directly on the article of food. The amount of insecticide shall not exceed exceed the tolerance limit prescribed in the food column.

Training Manual on Quality Assessment of Food Products

133

Note: *- on dry basis, **- on dried total solids basis, ***- on fat free substances, @ - on fat basis, @@ - on shell free basis, @@@ - on whole product basis, # - on carcass fat basis. 134 Training Manual on Quality Assessment of Food Products

PROCEDURE FOR PACKAGING OF VARIOUS FOOD PRODUCTS


Er. G. Velayudham
Assistant Professor, College of Food and Dairy Technology, Koduvalli, Chennai- 600 052.

The food safety and standard regulation 2011 has made vast conditions regarding the packaging and labeling of various food products and came into force in 05th august 2011. It explains about the general requirements, product specific requirements, specification of plastics packaging materials ,labelling, declaration regarding the food additives etc. GENERAL REQUIREMENTS 1. A utensil or container made of the following materials or metals, when used in the preparation, packaging and storing of food shall be deemed to render it unfit for human consumption. a. Containers which are rusty,

b. Enameled containers which have become chipped and rusty, c. Copper or brass containers which are not properly tinned,

d. Containers made of aluminium not conforming in chemical composition to IS:20 specification for wrought aluminium and aluminium alloy for utensils. 2. Containers made of plastic materials should conform to the following Indian standard specifications used as appliances or receptacles for packing or storing whether partly or wholly, food articles, namely a. IS: 10146Specification for polyethlene in contact with foodstuff

b. IS: 10142 Specification for styrene polymers in contact with foodstuff c. IS: 10151 Specification for polyvinylchloride in contact with food stuff

d. IS:10910Specification for polypropylene in contact with food stuff e. f. IS:11434Specification for ionomer resin in contact with food stuff. IS: 11704Specification for ethylene acrylic acid(EAA) copolymer.

g. IS:12252 Specification for poly alkylene terephathalates(PET) h. IS:12247Specification for nylon 6 polymer i. j. IS:13601Ethylene vinyl Acetate(EVA) IS:13576Ethylene metha acrylic acid(EMAA)

k. Tin and plastics containers once used, shall not be reused for packaging of edible oils and fats. 3. PACKAGING REQUIREMENTS OF CANNED PRODUCTS a.) All containers shall be securely packed and sealed. b.) The exterior of the cans shall be free from major dents, rust, perforations and seam distortions. c.) Cans shall be free from leaks.
Training Manual on Quality Assessment of Food Products 135

4. PACKAGING REQUIREMENTS FOR MILK AND MILK PRODUCTS a) Bottling or filling of containers with heat-treated milk and milk product shall be carried out mechanically and the sealing of the containers shall be carried out automatically. b) Wrapping or packaging may not be reused for dairy products, except where the containers are of a type which may be re-used after thorough cleaning and disinfecting. c) Sealing shall be carried out in the establishment in which the last heat-treatment of drinking milk or liquid milk base products has been carried out immediately after filling by means of a sealing device which ensures that the milk sealing is protected from any adverse effect of external origin on its characteristic. The sealing device shall be so designed that once the container has been opened, the evidence of opening remains clear and easy to check.

d) Immediately after packaging the dairy products shall be place in the rooms provided for storage. 5. PACKAGING REQUIREMENTS FOR EDIBLE OIL/FAT a.) Tin plate used for the manufacture of tin containers for packaging edible oils and fats shall conform to the standards of prime grade quality contained in B.I.S standards No.1993 or 13955 or 9025 or 13954 as amended from time to time and in respect of tin containers for packaging edible oils and fats shall conform to IS.No:10325 or 10339 as amended from time to time. 6. PACKAGING REQUIREMENTS FOR FRUITS AND VEGETABLES PRODUCTS a.) Every bottle in which any fruit product is packed shall be so sealed that it cannot be opened without destroying the licensing number and the special identification mark of the manufacture to be displayed on the top or neck of the bottle. b.) For canned fruits, juices and vegetables sanitary top cans made up of suitable kind of tin plates shall be used. c.) For bottled fruits, juices and vegetables only bottles/jars capable of giving hermetic seal shall be used. d.) Juices squashes, crush, cordials, syrups, barley waters and other beverages hall be packed in clean bottles securely sealed. These products when frozen and sold in the form of ice shall be packed in suitable cartons. Juices and pulps may be packed in wooden barrels when sulphited. e.) For packing preserves, jams jellies, and marmalades, new cans, clean jars, new canisters, bottle, chinaware jars, aluminium containers may be used and it shall be securely sealed. f.) For pickles, clean bottles, jars, wooden casks, tin containers covered from inside with polythene lining of 250gauge or suitable lacquered cans shall be used. g.) For tomato ketchups and sauces, shall be used. If acidity does not exceed 0.5% as acetic acid, open top sanitary cans may also be used. h.) Candied fruits and pels and dried fruits and vegetables can be packed in paper bags, cardboard or wooden boxes, new tins, bottle, jars, aluminium and other sutiable approved containers.

136

Training Manual on Quality Assessment of Food Products

i.) Fruits and vegetables products can also be packed in aseptic and flexible packaging material having food grade quality conforming to the standard laid down by BIS.\ 7. PACKAGING REQUIREMENTS FOR CANNED MEAT PRODUCTS: a.) New sanitary top cans made from suitable kind of tin plate shall be used. The cans shall be lacquered internally; they shall be sealed hermetically after filling. The lacquer used shall be sulphur resistant and shall not be soluble in fat or brine. b.) Cans used for filling pork luncheon meat shall be coated internally with edible gelatin, lard or lined with vegetable parchment paper before being filled. c.) Meat products packed in hermetically sealed containers shall be processed to withstand spoilage under commercial conditions of storage and transport. 8. PACKAGING REQUIREMENTS FOR DRINKING WATER(BOTH PACKAGED AND MINERAL WATER) a.) It shall be packed in clean, hygienic, colorless , transparent and tamperproof of bottles/containers made of polyethylene(PE)(Conforming to IS:10146 or polyvinyl chloride (PVC) conforming to IS:10151 or polyalkylene terephthalate(PET and PBT) conforming to IS:12252 or polypropylene conforming to IS:10910 or food grade polycarbonate or sterile glass bottles suitable for preventing possible adulteration or contamination of the water. All packaging materials of plastic origin shall as the prescribed overall migration and colour migration limits.

Training Manual on Quality Assessment of Food Products

137

138

Training Manual on Quality Assessment of Food Products

CHAPTER 6

Training Manual on Quality Assessment of Food Products

139

140

Training Manual on Quality Assessment of Food Products

FOOD BORNE DISEASES


Tmt.K.Sudha and V.Perasirian
Assistant Profesors,College of Food and Dairy Technology, Koduvalli, Chennai- 600 052.

Definition of Food borne diseases The term food borne disease is defined as a disease usually either infectious or toxic in nature, caused by agents that enter the body through the ingestion of food. Epidemiology Although food is a basic human need it can sometimes cause a number of illness arising from pathogenic and toxic substances, which find their way in to food through contamination or spoilage. Food borne illnesses have significant impact world wide including developed nations. The Center for Disease Control and Prevention (CDC) estimates for the US are 76 million cases, more than 300,000 hospitalization and 5000 deaths in a year. In addition 400 500 out breaks are reported. The spectrum of food borne diseases is constantly changing. New and re-emerging food-borne illnesses have resulted from recent changes in human demographics, international travel and commerce, microbial adaptations, economic development, technology and industry, eating behavior and land use. Classification and Etiology of Some Food Borne Diseases Food borne diseases are classified into two major categories depending on the causative agent: food-borne poisonings/intoxications and food-borne infections. Food borne infections: are diseases whose etiologic agents are viable pathogenic organisms ingested with foods and that can establish infection. Food borne poisonings/ intoxications: diseases arising from the ingestion of toxins released by microorganisms, intoxications from poisonous plants or toxic animal tissues: or due to consumption of food contaminated by chemical poisons. Food borne infections and foods commonly involved;

Training Manual on Quality Assessment of Food Products

141

142

Training Manual on Quality Assessment of Food Products

Food borne poisonings/intoxications and foods commonly involved;

Training Manual on Quality Assessment of Food Products

143

144

Training Manual on Quality Assessment of Food Products

PREVENTION AND CONTROL OF FOOD-BORNE DISEASES


Tmt.K.Sudha and V.Perasirian
Assistant Profesors, College of Food and Dairy Technology, Koduvalli, Chennai- 600 052.

Introduction The quality and safety of food is a topic of interest to the general public. Food quality from a more scientific point of view includes a number of safety aspects such as the presence of environmental contaminants, pesticide residues, and use of food additives, microbial contamination, and nutritional quality. In practical terms, safe food can be defined as food that, after being consumed, causes no adverse health effects. To ensure high quality of the food supply a number of parties must play specific roles. The main factors include the government, consumers, and the food industry. The government is responsible for the establishment of standards or codes of practice as well as the enforcement of laws and regulations. Furthermore, it should encourage the food industry to undertake voluntary measures to improve food safety. Consumers in turn should be well aware of the quality of the food they buy, prepare and consume and should adopt appropriate practices of food handling at home. At the industry level, all segments, including agriculture, should establish some system for safety assurance of their products and employ appropriate procedures and technologies. Adequate monitoring of food quality is usually more difficult to achieve. But, it is critical that preventive measures for ensuring food safety should be given great attention to prevent and or reduce food borne diseases. The following are possible preventive measures for ensuring food safety at various stages: 1. Production of raw materials To ensure safe food production, it is important to look at the agricultural level, where foods are initially produced, and improve the hygienic quality of raw foods. By improving the conditions under which crops, fruits, vegetables and food animals are raised, the hygienic quality of raw food products can be significantly improved. Furthermore, use of both pesticides and fertilizers should be reduced, and residue levels of toxic chemicals used to improve crop production should be systematically monitored. Prohibition of use of untreated sewage water for irrigation of vegetable fields is also an area of attention. Food safety at this stage can also be improved through measures aimed at reduction of industrial and vehicle emissions and disposal of hazardous waste materials that can enter the food chain. 2. Food Processing Greater demands are being made on the food-processing industry as a result of increasing urbanization. As consumers continue to move further a way from the sources of production, they will require an effective and safe food distribution system. This separation of the customer from the production sector means a loss of the traditional methods used by the consumer to ensure, the safety of food. Substantial losses of food by contamination and spoilage can be prevented through the use of carefully controlled technology and well designed food-processing infrastructure.
Training Manual on Quality Assessment of Food Products 145

The mainstay of microbiological food safety programs has been inspection. Inspection programs have serious limitations, however, as they sometimes over look critical factors that are not part of the inspection protocol. Inspection services are usually inadequate or non-existent in many developing countries in which Ethiopia is inclusive. A different approach to food safety in modern industrial food production and in food establishments is the Hazard Analysis and Critical Control Point (HACCP) system. This is an attempt to make a significant impact on the prevention of food-borne diseases. The HACCP system consists of a series of interrelated actions that should be taken to ensure the safety of all processed and prepared foods at critical points during the stages of production, storage, transport, processing, preparation, and service. 3. Food Preservation and Storage The aim of food preservation is to eradicate or prevent the growth of pathogens during manufacturing, processing and preparation of food so that it will remain, safe to eat for longer periods of time. Bacterial growth is enabled by a number of conditions, the most important being the presence of a good substrate (in this case a food item); an infection with viable organisms; a temperature that allows growth of bacteria; proper pH; and sufficient water for growth. To guard against microbial growth, at least one of these conditions should be hindrance. 4. Food Preparation in the Home The household is perhaps the most relevant place for developing strategies to combat food borne illness, as it is the location where the consumers, can exert the most control over what they eat. Clearly, one of the most significant components of keeping food pathogenfree in the household is maintaining a clean and hygienic environment in the kitchen or other food preparation areas. Proper sanitation facilities, cleanliness of household members who prepare the food, and control of pests are all essential for the presentation of acceptable food. Consumption cooked food; while still hot will not cause food borne infection. The chemical risks in food preparation at home are the same as those present during food processing. The general public should be made aware of these risks. Keeping chemicals away from kitchens and areas of food preparation is important. If needed, use chemicals cautiously. Many bacterial pathogens are able to multiply in food because of the temperature at which the food is stored. Figure 3.4.5 shows the temperatures at which bacteria can be killed or controlled. 5. Food preparation in the food service industry The consequences of improper food preparation in food services such as canteens and restaurants can be much greater than that in the household, simply because a large number of individuals may be simultaneously exposed to unsafe food items. It is essential to have a quality control program (inspection) that will ensure the maintenance of food product standards during all stages of handling, processing and preparation; it must also be applied to all areas and equipment that come into contact with food and beverages. Street foods are particularly prone to lapses in safe food preparation, hence requiring stringent control measures. The prevention and control strategies for food borne diseases emanate from the three basic principles (described in section3.4.4): the prevention of contamination, destroying the pathogenic agent or retarding the growth and multiplication of the biologic agent as well as retarding the production of toxins.
146 Training Manual on Quality Assessment of Food Products

Methods to keep food safe The art of keeping food safe and preservation requires knowledge of bacteria and the effect of the environment on microorganisms. Methods of keeping food safe and preservation include modern innovations such as vacuuming and filtration techniques, pressure canning and radiation processes. The primary objective of keeping food safe is to prevent food from acquiring hazardous properties during preparation, shipment, or storage. The principal methods and the techniques used to keep food safe include temperature control (including pasteurization, cooking, canning, and refrigeration, freezing and drying), fermentation and pickling, chemical treatment and irradiation. 1) Temperature control a). The use of high temperature Heat is one of the oldest methods of destroying microorganisms in food. The greatest advance in food hygiene was inadvertently made when man discovered the advantages of boiling, roasting, cooking and other heat treatments of food. Heat renders the destruction of microorganisms / pathogens and in some forms also destroys the toxin produced, such as in the case of the toxin of clostridium botulinum. Heat treatment may involve the following techniques.

Cooking / boiling / frying operations Blanching operations: Blanching is a mild pre-cooking operation involving brief scalding by hot water or steam, which is often used to reduce the bacterial load and insects on vegetable foods. Canning: This is the process of placing prepared (heat-treated) food in cans, exhausting the air from the cans, sealing the cans, sterilizing the sealed can and cooling it. Pasteurization: A process of heat treatment of food that kills pathogenic microorganisms without destroying taste, digestibility and nutritive value of food. It also destroys some food spoilage microorganisms. Drying (Desiccation): Bacteria cannot multiply in the absence of water (moisture). This can be achieved by application of heat or chemical treatment.

b). The use of low temperature Unlike high temperature, low temperature (cold) is not an effective means of destroying microorganisms and toxins in foods except retarding their multiplication and metabolic activities there by reducing toxin production.

Chilling (cold storage or refrigeration): is reducing food temperatures to below ambient temperatures. This is a suitable temperature to preserve perishable food items that may get spoiled at freezing temperature. Freezing: This is a dehydration method because the water in the food is transformed to ice, thus rendering it unavailable for microbial metabolic function. Freezing temperature depends upon the kind of food and the intended storage time.

Training Manual on Quality Assessment of Food Products

147

2). Fermentation and pickling In fermentation the food is transformed into an acid state based on the pH control principle. Some fermented foods have high amount of alcohol, which is antimicrobial. Pickling on the other hand refers to the immersion of certain foods in concentrated natural acid solution such as vinegar. 3). Chemical treatment This involves osmotic balance disturbance or direct actions of the chemicals on the microorganisms. Chemicals that increase osmotic pressure with reduced water activity below the level that permits growth of most bacteria can be used as bacteriostatic. Liquids pass into or out of bacterial cells by the process of osmosis. Examples for osmotic actions are salting and sugaring. Some other chemicals may destroy or inhibit growth of microorganisms in food. Examples include application of nitrites and smoking. 4). Radiation: this is a process of exposure of the food to high- speed electrons to destroy microbial cells. Beta, gamma or x-rays irradiate microorganisms in foods. A cell inactivated by irradiation cannot divide and produce visible growth (7). 5). Other important methods /supportive procedures that facilitate the safety of food

Health education Good personal and environmental hygiene Availability of safe, ample and convenient water supply Training of food handlers and managers Stringent inspection and control actions Legislative support (ordinances and codes), licensing Good-house keeping practices including separate storage and care of toxic chemicals. Understanding about additives and restrictions of unauthorized use. Food equipment selection to avoid chemical poisoning arising from the material constituency and or coatings of some food utensils. Avoidance and care of insecticide use in food processing and preparation areas.

148

Training Manual on Quality Assessment of Food Products

You might also like