Method Development and Validation of Analytical Procedures

Abstract

Method validation is the process used to confirm that the analytical procedure employed for a specific test is suitable for its intended use. Results from method validation can be used to judge the quality, reliability and consistency of analytical results; it is an integral part of any good analytical practice. It is the process of defining an analytical requirement, and confirms that the method under consideration has performance capabilities consistent with what the application requires. Use of equipment that is within specification, working correctly and adequately calibrated is fundamental to the method validation process. Likewise the operator carrying out the studies must be competent in the analysis under study and have sufficient knowledge of the method/analysis to draw conclusions from the observations as the validation work proceeds. Quite often method validation evolves from method development and so the two activities are often closely tied, with the validation study employing the techniques and steps in the analysis as defined by the method development. Analytical methods need to be validated or revalidated • before their introduction into routine use; • whenever the conditions change for which the method has been validated (e.g., an instrument with different characteristics or samples with a different matrix); and • whenever the method is changed and the change is outside the original scope of the method. Method validation has received considerable attention in the literature and from industrial committees and regulatory agencies. • The U.S. FDA CGMP request in section 211.165 (e) methods to be validated: The accuracy, sensitivity, specificity, and reproducibility of test methods employed by the firm shall be established and documented. Such validation and documentation may be accomplished in accordance with Sec. 211.194(a). These requirements include a statement of each method used in testing the sample to meet proper standards of accuracy and reliability, as applied to the tested product. The U.S. FDA has also proposed industry guidance for Analytical Procedures and Methods Validation. • ISO/IEC 17025 includes a chapter on the validation of methods with a list of nine validation parameters. The ICH has developed a consensus text on the validation of analytical procedures. The document includes definitions for eight validation characteristics. ICH also developed guidance with detailed methodology.