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Review Article
Email: kamal0603@gmail.com
Abstract:
Pharmaceutical analysis plays an important role right from testing of raw materials, inprocess quality checks to the analysis of finished products. Pharmaceutical analysis is
considered to determine identity, strength, quality and purity of drug samples. Pharmacists
have made important contributions in the field of medicinal chemistry, both in discovering or
isolating new therapeutic agents and in developing methods for standardizing and controlling
medicinal. In small laboratories the responsibility for performing analysis may be delegated
entirely to pharmacist staff members. But whether or not pharmacists may have occasion to
conduct analysis, they at least should understand the basic principles involved in the
standardization and control of the medicinal agents dispensed . The paper is focusing on the
parameters required to validate an analytical method.
Keywords : analytical chemistry, validation, limit of detection, limit of quantification,
robustness and ruggedness.
INTRODUCTION:
Analytical chemistry is as old as chemistry
itself. In many respect analytical chemistry
acts as a foundation for other branches of
chemistry. In fact, the science of chemistry
came into being as a result of human
inquisitiveness to understand the nature of
an extraordinary variety of matter that
surrounds him. In analytical chemistry it is
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Benefits of Validation
a) Produces quality products
b) Helps in process improvement
technology transfer, related product
validation, failure investigation, and
increased employee awareness.
c) Cost reduction by increasing
efficacy,
few
reject,
longer
equipment life, production of cost
effective products
d) Helps in optimization of process or
method.
e) Regulatory
affairs-produces
approved products and increased
ability to export.
The US Food and Drug Administration
(FDA) [8-9] and US Pharmacopoeia
(USP) [10] both refer to ICH guidelines.
Validation as Defined by Different
Agencies[11]
EUROPEANCOMMITTEE:
Defines Validation as an action of
providing in accordance with the
principles of GMP that any procedure.
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2.
Visual evaluation (relevant
chromatogram acceptable)
3.
The standard deviation of
the response and the slope.
LOD =
3.3
S
= Standard deviation of
the response.
S = Slope of the calibration
curve of the analyte
Limit of Quantification
The LOQ is the lowest concentration of
analyte in a sample which can quantitative
determined that may be measured with an
acceptable level of accuracy and precision
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LOQ =
10
S
= Standard deviation of
the response.
S = Slope of the
calibration curve of the analyte
Measurement
For instrumental and non instrumental
methods the quantitation limit is
generally determined by the analysis of
the samples with known concentration of
the analyte and by establishing the
minimum level at which the analyte can
be determined with acceptable accuracy
and precision.
In case of instrumental methods that
exhibit back ground noise the ICH
document
describes
to
compare
measured signals from samples with
known concentration of analyte with
those of blank samples.
A typically acceptable signal to noise
ratio is 10:1
Ruggedness
Degree of reproducibility of test results
obtained by analyzing the same sample
under variety of normal test conditions
such as different.
Analysts
Instruments
Days
Reagents
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