Journal of Chromatography Library Series

Bioaffinity chromatography has increasingly become the method of choice for the purification, determination or removal of many biologically active substances.

Porous Silica

Chemical Derivatization in Gas Chromatography

This multi-author volume provides an unprecedented in-depth coverage of the separation, identification and quantitation of simple and complex food and tissue fats and other lipids by chromatographic and mass spectrometric methods with emphasis on applications to biomedical research and clinical diagnosis. It contains a total of 13 chapters written by scientists who are internationally recognized in their specific fields. The volume covers analyses of molecular species of eicosanoids, sterols, and glycero and glycolipids in healthy and diseased human tissues and in appropriate animal models. The text complements the simpler group determinations of lipid classes commonly employed in clinical laboratories. The volume anticipates the discovery of the specific metabolism of molecular species of complex glycerolipids and provides the medical researcher and clinical investigator with the means for dealing with it.

The rapid development of new packings for aqueous size-exclusion chromatography has revolutionized this field. High resolution non-adsorptive columns now make possible the efficient separation of proteins and the rapid and precise determination of the molecular weight distribution of synthetic polymers. This technology is also being applied to the separation of small ions, the characterization of associating systems, and the measurement of branching. At the same time, fundamental studies are elucidating the mechanisms of the various chromatographicprocesses. These developments in principles and applications are assembled for the first time in this book. Fundamental issues are dealt with: the roles of pore structure and macromolecular dimensions, hydrophobic and electrostatic effects, and the determination and control of column efficiency. High-performance packings based on derivatized silica are reviewed in detail. Special techniques are thoroughly described, including SEC/LALLS, inverse exclusion chromatography, and frontal zone chromatography. Attention is focussed on special applications of size-exclusion methods, such as the characterization of micelles, separations of inorganic ions, and Hummel-Dreyer and related methods for equilibrium systems. Protein chromatography is dealt with in both dedicated sections and throughout the book as a whole. This is a particularly comprehensive and authoritative work - all the contributions review broad topics of general significance and the authors are of high repute. The material will be of special value for the characterization of synthetic water-soluble polymers, especially polyelectrolytes. Biochemists will find fundamental and practical guidance on protein separations. Researchers confronted with solutes that exhibit complex chromatographic behavior, such as humic acids, aggregating proteins, and micelles should find the contents of this volume illuminating.

Electron Capture

Gradient Elution in Column Liquid Chromatography

This book gives a comprehensive, up-to-date review of all selective detectors used in combination with gas chromatography. For each detector, the historical background, design and principle are described, and the working parameters affecting the detector performance are analyzed critically and in detail. The analytical possibilities of the detectors and the main characteristics such as sensitivity, noise and minimum detectability are discussed. All the selective detectors that are currently used are discussed in detail. Combinations of GC with other techniques such as plasma emission spectroscopy, atomic absorption spectrometry, ion-selective electrodes, piezoelectric sorption detector, mass spectrometry and infrared spectroscopy are discussed briefly. Chromatographers and users of gas chromatographs, especially in the field of environmental protection, agriculture, clinical chemistry, and toxicology will find the book useful to their work. Institutes and organisations dealing with analytical chemistry will also find it of interest.

The renaissance of liquid chromatography took place in the late 1960's and early 1970's. The first edition of this book published in 1977 described the detectors that were available at that time and which provided a performance matching that of the contemporary equipment with which they were associated. It is interesting to note that the most popular detectors then (the UV detector, the refractometer detector, the fluorescence detector and the electrical conductivity detector) are still the most commonly used detectors nearly a decade later. Detector design, however, has changed very significantly over the intervening years. Modern high efficiency columns provide very narrow peaks and very fast separations, and thus the physical design of the detectors had to change to meet these new challenges. In 1977, there was little real understanding of the important role played by the detector in the overall function of the chromatographic system and although some of the factors were pointed out in the first edition of this book, in retrospect they appeared to be little understood. This second edition gives an entirely new presentation of the subject of liquid chromatography detectors. It contains sections dealing with the fundamental aspects of the interaction between columns and detectors and the interaction between ancillary equipment and the detector. It brings the reader up-to-date with new designs and novel detecting systems that have been developed since 1977 and extends significantly the subject of the association of the liquid chromatography detector with spectroscopic techniques. In particular the book now explores the association of liquid chromatography with nuclear magnetic resonance, infrared and atomic absorption spectrometry. This book not only gives a comprehensive treatment of the subject of liquid chromatographic detectors and provides a rational procedure for defining their performance and so permit valid comparisons, but also discusses detector performance in relation to the whole of the chromatographic system.

The main subject of this book is the characterization of plastics. To a high degree the properties of these polymers depend on the distribution of the molar mass and of other structural features, and small deviations frequently have a great effect. Therefore the characterization of polymers cannot be restricted to the determination of mean values but must yield information on these distributions. Using classical methods, the analytical fractionation of polymer homologues and structurally isomeric polymers is extremely time-consuming. Therefore, efficient chromatographic techniques are being increasingly employed in modern polymer characterization. In the first place, high-performance liquid chromatography is applied, in the form of size exclusion chromatography. It is also possible, however, to use other separation modes. More space is devoted to these other possibilities in this volume than is merited by their current range of applications, as the author believes that many separation problems will be solved by separation techniques of the non-exclusion type. Nevertheless, much emphasis is placed on size exclusion chromatography. Not only because of its current wide range of applications, but also because its relative importance, as a complement to other chromatographic techniques may even increase in the forthcoming years. This book is the first to cover all phenomena related to the above considerations. Starting with an introduction to basic liquid chromatography and to polymer science, it deals with the adsorption behaviour of polymers, with gradient techniques, with the kinetic band broadening in liquid chromatography, with instrumental features and packing materials. The book consists of four balanced sections and related information from about 1800 references is compiled in the tables. Some 250 figures and 30 tables will help give the reader a clear insight of the topics discussed. The book is aimed at helping the analyst or polymer chemist who is looking for information about chromatographic methods for the characterization of polymers.

Here is an invaluable new book on quantitative gas chromatography which explains how the method can - or should - be used for accurate and precise analysis. Gas chromatography is firmly established as one of the few major methods for the quantitative analysis of complex mixtures. It is fast, accurate and inexpensive, with a broad range of applications. It has however become very complex and involved: over 200 stationary phases, more than 10 detector principles and several very different column types are available from among the catalogs of over 100 manufacturers and major retailers. The progressive changes in the nature of gas chromatography have created new needs for information which are not satisfied by the literature presently available. This book provides a complete discussion of all the problems involved in the achievement of quantitative analysis by gas chromatography, whether in the research laboratory, in the routine analysis laboratory or in process control. For this reason the presentation of theoretical concepts has been limited to the essential, while extensive explanations have been devoted to the various steps involved in the derivation of precise and accurate data. This starts with the selection of the instrumentation and column, continues with the choice of optimum experimental conditions, then calibration and ends with the use of correct procedures for data acquisition and calculations. Finally, there is almost always a way to reduce errors and an entire chapter deals with this single issue. Numerous relevant examples are presented. The first part of the book presents the theoretical background, simple enough to be understood by all analytical chemists, but still complete and up-to-date. It discusses the problems of flow dynamics, retention and band broadening. The changes in band profile associated with column overloading are explained without much recourse to mathematics. The second part describes the gas chromatograph and discusses the properties of each of its parts: gas flow and pressure controller sampling system, oven, column switching valves, detectors. The different implementations, their advantages and drawbacks are discussed and compared. In addition, three chapters present packed column technology, open tubular column technology and some sophisticated new phase systems, respectively. The new phase systems described use adsorbents, modified by coating or grafting organic phase, and carrier gases containing vapors which are sorbed by the stationary phase and modify it, such as steam. The third part discusses the applications in qualitative and quantitative analysis. Calibration, peak integration, sources of errors arising from the various parts of the instrument as well as from the measurement process itself are carefully described in four detailed chapters. Methods to carry out accurate and precise analysis are presented. A last chapter is devoted to process control analysis and gives a number of detailed examples of applications. A lexicon explaining the most important chromatographic terms and a detailed index complete the book. This is a book which no chemical analyst should be without. It should be on the library shelf of all universities, instrument companies and any laboratory and plant where gas chromatography is used.

This volume provides a straightforward approach to isolation and purification problems with a thorough presentation of preparative LC strategy including the interrelationship between the input and output of the instrumentation, while keeping to an application focus. The book stresses the practical aspects of preparative scale separations from TLC isolations through various laboratory scale column separations to very large scale production. It also gives a thorough description of the performance parameters (e.g. throughput, separation quality, etc.) as a function of operational parameters (e.g. particle size, column size, solvent usage, etc.). Experts in the field have contributed a well balanced presentation of separation development strategies from preparative TLC to commercial preparative process with practical examples in a wide variety of application areas such as drugs, proteins, nucleotides, industrial extracts, organic chemicals, enantiomers, polymers, etc.

Capillary Electrophoresis (CE) has had a very significant impact on the field of analytical chemistry in recent years as the technique is capable of very high resolution separations, requiring only small amounts of samples and reagents. Furthermore, it can be readily adapted to automatic sample handling and real time data processing. Many new methodologies based on CE have been reported. Rapid, reproducible separations of extremely small amounts of chemicals and biochemicals, including peptides, proteins, nucleotides, DNA, enantiomers, carbohydrates, vitamins, inorganic ions, pharmaceuticals and environmental pollutants have been demonstrated. A wide range of applications have been developed in greatly diverse fields, such as chemical, biotechnological, environmental and pharmaceutical analysis. This book covers all aspects of CE, from the principles and technical aspects to the most important applications. It is intended to meet the growing need for a thorough and balanced treatment of CE. The book will serve as a comprehensive reference work. Both the experienced analyst and the newcomer will find the text useful.

The aim of this volume is to describe the most recent advances in areas of analytical chemistry that relate to the trace determination of metals and inorganics, as well as their distribution and forms (species) present, sample dependent. Analytical approaches are described that encompass a number of separation methods, such as gas and high performance liquid chromatography, interfaced with selective and sensitive detection methods that become unique for metal species/forms present in various samples. Hyphenated techniques are emphasized, such as interfacing HPLC with plasma induced emission spectroscopy, electrochemistry, post-column reaction chemistry, etc. Each chapter describes the latest instrumental and methodology advances that utilize some form of chromatography together with element-specific detection or mass spectrometry to provide absolute identification of the specific species of a metal present in various samples. The book will be of value to those concerned with the determination of trace levels of individual metal species present or suspected present in any given sample and to those involved in trace metal toxicology, metabolism of metal-containing drugs or chemicals, environmental exposures to metals and chemical speciation of real world samples. Government regulatory laboratories striving to detect and determine absolute levels of a metal species in any regulated sample will be interested in this volume, as will academic institutes involved in environmental toxicology, environmental chemistry, metal-DNA/protein interactions and researchers working with metal species.

This new book encompasses, in great detail, the most recent progress made in the isolation and separation of natural products. It covers antibiotics, marine and plant-derived substances, enzyme inhibitors and interferons. The most recent separation methodology is described. Although there is a bias toward antibiotics, it was done because this is still the largest natural products area of research. The fourteen chapters are written by experts in their respective fields. The first two chapters are largely devoted to new methodology applied to purification of a variety of compounds. They include an extensive review and new applications of counter-current chromatography and the newly emerging HPLC-photodiode array technology. Chapter 3 provides a review of affinity chromatography applied to the separation of antibiotics for the first time. Next are chapters on antimicrobials with an update on all the most recent -lactam (after 1976) discoveries. A comprehensive review of a very important class of antiparasitic agents - the avermectins - follows. An update of isolation and purification of a variety of marine-derived compounds is next. The succeeding chapter is a comprehensive review of the most recent developments in isolation and purification of interferons. This is followed by a discussion of enzyme inhibitors and their isolation and purification and ties in with a chapter on plant-derived natural products, some of which are also in this same category. The final chapter is a futuristic essay indicating the isolation of minute amounts of natural products and the fascinating biological properties which they possess. The book has extensive isolation schemes, tables, figures and chemical structures. In many instances a short summary of the producing organism, brief chemical description and structure and biological activity of the compounds is presented. Detailed information of extraction, separation and purification techniques follow. Each chapter has an extensive bibliography and, where applicable, an appendix showing sources of materials and equipment. A detailed index to the subject matter is included at the end of the book. The book thus offers the reader: up-to-date reviews (including 1988) of specific topics in the natural products field not to be found elsewhere; information on new chromatographic methods and techniques described in sufficient detail to be utilized by investigators in this area of research; and extensive references to enable the serious researcher to pursue particular information. It will appeal to pharmaceutical and natural products researchers and is a valuable acquisition for university chemistry and biochemistry departments.

Carbohydrates and glycoconjugates play an important role in several life processes. The wide variety of carbohydrate species and their inherent polydispersity and heterogeneity require separation techniques of high resolving power and high selectivity such as high performance liquid chromatography (HPLC) and capillary electrophoresis (HPCE). In the last decade HPLC, and recently HPCE methods have been developed for the high resolution and reproducible quantitation of carbohydrates. Despite the importance of these two column separation technologies in the area of carbohydrates, no previous book describes specialized methods for the separation, purification and detection of carbohydrates and glycoconjugates by HPLC and HPCE. Therefore, the objective of the present book is to provide a comprehensive review of carbohydrate analysis by HPLC and HPCE by covering analytical and preparative separation techniques for all classes of carbohydrates including mono- and disaccharides; linear and cyclic oligosaccharides; branched heterooligosaccharides (e.g., glycans, plant-derived oligosaccharides); glycoconjugates (e.g., glycolipids, glycoproteins); carbohydrates in food and beverage; compositional carbohydrates of polysaccharides; carbohydrates in biomass degradation; etc. The book will be of interest to a wide audience, including analytical chemists and biochemists, carbohydrate, glycoprotein and glycolipid chemists, molecular biologists, biotechnologists, etc. It will also be a useful reference work for both the experienced analyst and the newcomer as well as for users of HPLC and HPCE, graduates and postdoctoral students.

This encyclopaedic catalogue of the pitfalls and problems that all analysts encounter in their work is destined to spend more time on the analyst's workbench than on a library shelf. The author has dedicated the book to ``the innumerable scientists who made mistakes, used impure chemicals and solvents, suffered the consequences of unanticipated side-reactions, and were otherwise exposed to mayhem yet were not too embarrassed to publish their findings''. Traditionally, the mass spectroscopist or gas chromatographer learnt his trade by participating in a 4-6 year apprenticeship as graduate student and post-doctoral researcher. Generally, no formal training was provided on the things that go wrong, but this information was accumulated by sharing in the experiences of colleagues. Nowadays, many novice scientists simply purchase a computerized instrument, plug it in, and use it. Much time can be wasted in studying and resolving problems due to artifacts and there is also a strong possibility that artifacts will not be recognized as such. For example, most analysts realize that they should use glass rather than plastic containers; but few of them would anticipate the possibility of plasticizer residues on glassware washed using detergent from a plastic bottle. This book is an easy-to-use compendium of problems encountered when using various commonly used analytical techniques. Emphasis is on impurities, by-products, contaminants and other artifacts. A separate entry is provided for each artifact. For specific chemicals, this entry provides the common name, mass spectrum, gas chromatographic data, CAS name and registry number, synonyms and a narrative discussion. More than 1100 entries are included. Mass spectral data are indexed in a 6-peak index (molecular ion, base peak, second peak, third peak) and there are also formula, author and subject indexes. An extensive bibliography contains complete literature citations. The book is designed to be used. It will not only allow experienced analysts to profit from the mistakes of others, but it will also be invaluable to other scientists who use analytical instruments in their work.

The primary aim of this volume is to make the chemist familiar with the numerous stationary phases and column types, with their advantages and disadvantages, to help in the selection of the most suitable phase for the type of analytes under study. The book also provides detailed information on the chemical structure, physico-chemical behaviour, experimental applicability, physical data of liquid and solid stationary phases and solid supports. Such data were previously scattered throughout the literature. To understand the processes occurring in the separation column and to offer a manual both to the beginner and to the experienced chromatographer, one chapter is devoted to the basic theoretical aspects. Further, as the effectiveness of the stationary phase can only be considered in relation to the column type, a chapter on different column types and the arrangement of the stationary phase within the column is included. The secondary aim of this book is to stimulate the development of new and improved standardized stationary phases and columns, in order to improve the reproducibility of separations, as well as the range of applications.

This book brings together a number of studies which examine the ways in which the retention and selectivity of separations in high-performance liquid chromatography are dependent on the chemical structure of the analytes and the properties of the stationary and mobile phases. Although previous authors have described the optimisation of separations by alteration of the mobile phase, little emphasis has previously been reported of the influence of the structure and properties of the analyte. The initial chapters describe methods based on retention index group increments and log P increments for the prediction of the retention of analytes and the ways in which these factors are influenced by mobile phases and intramolecular interactions. The values of a wide range of group increments in different eluents are tabulated. Different scales of retention indices in liquid chromatography are described for the comparison of separations, the identification of analytes and the comparison of stationary phases. Applications of these methods in the pharmaceutical, toxicology, forensic, metabolism, environmental, food and other fields are reviewed. The effects of different mobile phases on the selectivity of the retention indices are reported. A compilation of sources of reported retention index values are given. Methods for the comparison of stationary phases based on the interactions of different analytes are covered, including lipophilic and polar indices, shape selectivity comparisons, their application to novel stationary phases, and chemometric methods for column comparisons.

This book presents a guide for the analysis of biomedically important compounds using modern liquid chromatographic techniques. After a brief summary of basic liquid chromatographic methods and optimization strategies, the main part of the book focuses on the various classes of biomedically important compounds: amino acids, catecholamines, carbohydrates, fatty acids, nucleotides, porphyrins, prostaglandins and steroid hormones. The different chapters discuss specialized techniques pertaining to each class of compounds, such as sample pretreatment, pre- and post-column derivatization, detection and quantification.

Air pollution determination is one of the most important fields of gas chromatography application in practice. This book provides a systematic description of the main stages of air pollution determination, ranging from sampling problems to the quantitative estimation of the acquired data. Special attention is paid to the problem of gas, vapor, spray and solid particles extraction from air. The main methods of sampling procedure, namely, container utilization, cryogenic concentration, absorption, adsorption, chemisorption and filter usage, and successive impurities extraction are also handled. Sorption theory and the problems of sorption and desorption efficiency for hazardous impurities being extracted from traps with sorbents are discussed in detail. The practical utilization of different sorbents (silica, activated carbon, polymers etc.) to carry out sampling procedures for 200 main pollutants with known TLV (USSR and USA) is also considered. This highly informative book, reflecting several insufficiently known techniques as well as the experience of both western and Soviet researchers, should be of interest to both beginners and skilled researchers.

This is the first book to focus on the latest developments in hyphenated techniques using supercritical fluids. The advantages of SFC in hyphenation with various detection modes, such as FTIR, MS, MPD and ICP and others are clearly featured throughout the book. Special attention is paid to coupling of SFE with GC or SFC. In this edited volume, chapters are written by leading experts in the field. The book will be of interest to professionals in academia, as well as to those researchers working in an industrial environment, such as analytical instrumentation, pharmaceuticals, agriculture, food, petrochemicals and environmental.

This work comprises two parts, Part A: Techniques and Part B: Applications. In Part A the most important principles of sample preparation, extraction, clean-up, and of established and prospective chromatographic techniques are discussed in relation to mycotoxins. In Part B the most important data, scattered in the literature, on thin-layer, liquid, and gas chromatography of mycotoxins have been compiled. Mycotoxins are mostly arranged according to families, such as aflatoxins, trichothecenes, lactones etc. Chromatography of individual important mycotoxins and multi-mycotoxin chromatographic analyses are also included. Applications are presented in three chapters devoted to thin-layer, liquid, and gas chromatography of mycotoxins.

It is widely recognized that analytical technologies and techniques are playing a pioneering role in a range of today's foremost challenging scientific endeavours, including especially biological and biomedical research. Worthy of mention, for example, are the role that high performance separation techniques played in mapping the human genome and the pioneering work done within mass spectrometry. It is also apparent that state-of-the-art pharmaceutical and biomedical research is the major driving force of the development of new analytical techniques. Advancements in genomics research has provided the opportunity for a call for new drug targets for new technologies, which has speeded up drug discovery and helped to counteract the trend towards inflation of R&D costs. This book has been designed to be a reference covering a wide range of protein and genomic material analysis techniques. Emerging developments are presented with applications where relevant, and biological examples are included. It was developed to meet the ever growing need for a comprehensive and balanced text on an analytical technique which has generated a tremendous amount of interest in recent years. In addition, this book also serves as a modern textbook for advanced undergraduate and graduate courses in various disciplines including chemistry, biology and pharmacy. Authors of the individual chapters are recognized champions of their individual research disciplines and also represent contemporary major research centres in this field. · Contains state-of-the-art knowledge of the field and detailed descriptions of new technologies · Provides examples of relevant applications and case studies · Contributing authors are leading scientists in their own respective research fields

Bioaffinity chromatography is now the preferred choice for the purification, determination or removal of many biologically active substances. The book includes information on biologically active substances with their affinants, solid supports and methods of coupling, summarized in tables covering classical, high-performance liquid and large-scale bioaffinity chromatography. Optimization of the preparation and the use of highly active and stable biospecific adsorbents is discussed in several chapters. Following a chapter dealing with the choice of affinity ligands, affinity-sorbent bonding is described in detail. Other chapters give information on solid supports, the most common coupling procedures and a general discussion of sorption and elution. Several applications of bioaffinity chromatography are described, e.g. quantitative evaluation of biospecific complexes and many applications in medicine and in the biotechnology industry.

The different LC-MS techniques available today were developed to suit specific analytical needs and the application range covered by each one is wide, but still limited. GC amenable compounds can be all analyzed with a single GC-MS system whereas HPLC applications call for specific LC-MS instrumental arrangements. ESI, APCI, APPI, and EI are ionization techniques that can be combined with different analyzers, in single or tandem configuration, to create the ultimate system for a certain application. Once approaching LC-MS for a specific need, the fast technical evolution and the variegated commercial offer can induce confusion in the potential user. The role of this book is to enlighten the state-of-the-art of LC-MS evolution through a series of contributions written by the people that brought major, recent innovations in the field. Each chapter will take into consideration the novelties, the advantages and the possible applications covered by a particular technical solution. The book will also include new analytical methods that can provide benefits using the most recent innovations in LC-MS plus a certain number of key applications. - Contains contributions from major innovators in the field - Covers the latest developments in the field of LC-MS - Gives a clear outline on the advantages of various techniques and their applications