Analytical Method Validation Principles and Practices

Chung Chow Chan, Azopharma Contract Pharmaceutical Services, Miramar, Florida, Analytical Method Validation Principles and Practices... 

J.D. MacNeU, J. Patterson, and V. Martz, Validation of analytical methods - proving your method is fit for purpose, in Principles and Practices of Method Vahdation, ed. A. Flajgelj and A. Ambrus, MPG Books, Bodmin, pp. 100-107 (2000). 

R. Caulcutt and R. Boddy, Statistics for Analytical Chemists, Chapman and Hall, London, 1983. A. Fajgelj and A. Ambras, Eds., Principles and Practices of Method Validation, The Royal Society of Chemistry, Cambridge, UK, 2000. 

Guidelines for single-laboratory validation of analytical methods for trace-level concentrations of organic chemicals. In Fajeli A, Ambrus A, editors. Principles and practices of method validation. Cambridge, England Royal Society of Chemistry 2000. p. 179-252. 

Recently, major developments in statistical methods have been made particularly in the areas of collaborative studies and method validation and robustness testing. In addition, analytical method development and validation have assumed a new importance. However, this handbook is not intended to be a list of statistical procedures but rather a framework of approaches and an indication of where detailed statistical methods may be found. Whilst it is recognised that much of the information required is available in the scientific literature, it is scattered and not in a readily accessible format. In addition, many of the requirements are written in the language of the statistician and it was felt that a clear concise collation was needed which has been specifically written for the practising analytical chemist. This garnering of existing information is intended to provide an indication of current best practices in these areas. Where examples are given the intent is to illustrate important points of principle and best practice. 

This document was updated and replaced in 2009 by CAC/GL 71-2009. This new document introduced a number of major revisions to previous practice, particularly the introduction of performance criteria for analytical methods and the principle of single-laboratory validation. In the earlier document, analytical methods were accepted by the CCRVDF only if they had been fully validated by a rigorous multi-laboratory collaborative trial. Experience within the CCRVDF had shown that it was becoming increasingly difficult to organise such trials, and many laboratories were adopting performance criteria to validate analytical methods. 

Elucidation of how the general principles underlying the concept of validation should be expressed in practice is an evolving process, as exemplified by the ongoing evolution of validation requirements for bioanalytical assays in the pharmaceutical industry (Shah 1992, 2000 FDA 2001 Viswanathan 2007). The complementary principle of fitness for purpose (Section 9.2) applies not only to the assay method but also to the validation process itself. Procedures that are considered to be fit for purpose in validation of an analytical method to be used in drug development, for example, need not necessarily apply to, e.g., methods used to screen pesticide residues in foodstuffs. As noted in Section 9.2, this point of view appears to be consistent with the definition of validation applied to all measurements (ISO 1994) Validation Confirmation by examination and provision of objective evidence that the particular requirements for a specified intended use are fulfilled. Of course, some basic principles are common to all validation schemes. 

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