国际上不同分析方法验证准则综述.pptVIP

483 Observations There was inadequate method validation specificity data to demonstrate that each method was capable of distinguishing the active ingredient from its impurities and degradation products. Specificity studies did not include the minimum stress conditions of acid and base hydrolysis, oxidation, thermal degradation and photolysis, degradation schematic for the active ingredient that identifies the major degradation products was not included for each product. * 2009 FDA Waning Letter On addition to the example of modifying both compendial methods and customer supplied methods, we also observed the use of unvalidated in-house methods as well as unvalidated modifications to in-house methods. A statement indicating that the method has not been validated in the particular formulation was included in the certificate of analysis for…use of this statement does not absolve…from using valid, accurate, and reproducible methods. (June 2000) * 2009 FDA Systems Based Inspection:Laboratory System * Method Validation 13% Training/Qual. 4% Stability Program 21% Inadequate Records 27% Controls. General 35% Feb – July 2002: 212 Inspections (US) * Reference: Albinus D’ Sa, FDA, CDER Office of Compliance, from AAPS, Nov. 2002 presentation. 2009 Related Site /cder/ * * * * * 国际上不同分析方法验证的准则概述 7/8/2010 蔡磊明 分析方法验证是论证某一分析方法适用于其用途的过程。 Analytical method validation is the process to confirm that the analytical procedure employed for a specific test is suitable for its intended use. 分析方法验证Method Validation 7/8/2010 Slide * Criteria for Method Validation Limit of detection Limit of quantitation Precision (Intermediate precision) Accuracy Linearity/Range Selectivity/Specificity Ruggedness Robustness Actual validation effort depends on the analysis problem Proof suitability for intended use Definition Method Scope Define Validation Criteria Test Define Routine Tests Validation of Analytical Methods Sample matrix Compounds Equipment, Location Optimize method para