Step-by-Step Analytical Methods Validation and Protocol in the Quality System Compliance Industry

Method validation is an important requirement for any package of information submitted to international regulatory agencies in support of new product marketing or clinical trials applications. Analytical methods should be validated, including methods published in the relevant pharmacopoeia or other recognized standard references. The suitability of all test methods used should always be verified under the actual conditions of use and should be well documented. Methods should be validated to include consideration of characteristics included in the International Conference on Harmonization (ICH) guidlines 1, 2 addressing the validation of analytical methods. Analytical methods outside the scope of the ICH guidance should always be validated. ICH is concerned with harmonization of technical requirements for the registration of products among the three major geographical markets of the European Community (EC), Japan, and the United States (U.S.) of America. The recent U.S. Food and Drug Administration (FDA) methods validation guidance document, 3-5 as well as the United States Pharmacopoeia (USP), 6 both refer to ICH guidelines. The most widely applied typical validation characteristics for various types of tests are accuracy, precision (repeatability and intermediate precision), specificity, detection limit, quantitation limit, linearity, range, and robustness (Figure 1). In addition, methods validation information should also include stability of analytical solutions and system suitability. 7