Methods of validating a test instrument

30-Sep-2017 07:35

The literature contains diverse approaches to performing validations (as in References 6--10).This Report presents an approach to performing validation studies that encompasses much of the current literature and provides practical guidance.The process of method development and validation has a direct impact on the quality of these data.Although a thorough validation cannot rule out all potential problems, the process of method development and validation should address the most common ones.The remaining studies are performed when the drug reaches the Phase III (efficacy) stage of development and has a higher probability of becoming a marketed product.The process of validating a method cannot be separated from the actual development of the method conditions, because the developer will not know whether the method conditions are acceptable until validation studies are performed.The response of the analyte in test mixtures containing the analyte and all potential sample components (placebo formulation, synthesis intermediates, excipients, degradation products, process impurities, etc.) is compared with the response of a solution containing only the analyte.Other potential sample components are generated by exposing the analyte to stress conditions sufficient to degrade it to 80-90% purity.

The resulting mixtures are then analyzed, and the analyte peak is evaluated for peak purity and resolution from the nearest eluting peak.In general, methods for regulatory submission must include studies on specificity, linearity, accuracy, precision, range, detection limit, quantitation limit, and robustness.