HPLC方法验证及方案.pdf

HANDBOOK OF GENERIC DRUG DEVELOPMENT info@iagim.org ANDA DEVELOPMENT SECTION XV SECTION 15 Analytical Methods (TYPICAL ANALYTICAL METHOD VALIDATION) 1. PURPOSE The purpose of this Standard Analytical Procedure is to demonstrate the procedure required to validate in-house HPLC analytical methods and to show that the methods are stability-indicating. Methods based on the USP but modified for stability indicating test purposes require full in-house validation. This procedure ensures that the Product Development Process and Process Qualification Batch analysis is based on a foundation of Good Laboratory Practice using validated test procedures. 2. RESPONSIBILITY The Head of Analytical Development in coordination with the managers of QC and Regulatory Affairs at the proposed manufacturing site. 3. FREQUENCY For each non-compendial analytical method intended for ANDA (or OTC ANDA) manufactured products. For Stability-Indicating Assays and limit testing of impurities that may be based on compendial methods. Each Product strength will follow the full method validation procedure. 4. PROCEDURE [a]. Method Validation Non-compendial methods validation will follow the USP direction for parameters needed for the validation of test methods. Typical parameters for validating assays and other non-compendial analytical methods designed for providing quantitative results shall include : Accuracy Recovery Precision ( System reproducibility, Method reproducibility ) Specificity Linearity Range Ruggedness (different analysts / days /different equipment models / columns) [b]. Placebo Analysis. A mixture of non-actives (placebo) shall be prepared and subjected to analysis