Front Cover -- Specification of Drug Substances and Products: Development and Validation of Analytical Methods -- Copyright -- Contents -- List of Contributors -- Part 1 - Introduction -- Chapter 1 - Introduction -- References -- Chapter 2 - General principles and regulatory considerations: specifications -- 2.1 DEFINITIONS -- 2.2 SPECIFICATION SETTING PROCESS -- 2.3 CERTIFICATES OF ANALYSIS, TRENDING AND OOS RESULTS -- 2.4 SPECIFICATIONS IN EARLY DEVELOPMENT -- References -- Chapter 3 - Application of quality by design (QbD) to the development and validation of analytical methods -- 3.1 INTRODUCTION -- 3.2 METHOD REQUIREMENTS -- 3.3 METHOD RISK ASSESSMENT -- 3.4 METHOD DEVELOPMENT AND OPTIMIZATION: UNDERSTANDING THE METHOD OPERATING SPACE -- 3.5 EMPIRICAL MODELS: DOE (SCREENING, MODELING, ROBUSTNESS) -- 3.6 APPROACHES USING EXPLICIT MODELS -- 3.7 GENERAL ADVICE ON DESIGN/ANALYSIS OF EXPERIMENTS -- 3.8 CASE STUDY-SAMPLE EXTRACTION METHOD DEVELOPMENT USING A RESPONSE SURFACE DESIGN -- 3.9 DEVELOPMENT TO VALIDATION -- 3.10 KNOWLEDGE MANAGEMENT -- 3.11 QBD THROUGHOUT THE METHOD LIFETIME -- 3.12 CONCLUSIONS -- References -- Chapter 4 - General principles and regulatory considerations: method validation -- 4.1 INTRODUCTION -- 4.2 DEFINITIONS -- 4.3 GUIDELINES -- 4.4 PHASE APPROPRIATE METHOD VALIDATION -- 4.5 VERIFICATION OF COMPENDIAL METHODS -- 4.6 REVALIDATION OF METHODS -- 4.7 METHOD REMEDIATION -- 4.8 METHOD TRANSFER -- References -- Part 2 - Universal Tests -- Chapter 5 - Description and identification -- 5.1 INTRODUCTION -- 5.2 DESCRIPTION -- 5.3 DRUG SUBSTANCE IDENTIFICATION TESTING -- 5.4 DRUG PRODUCT IDENTIFICATION -- 5.5 SUMMARY -- References -- Chapter 6 - Assay and impurities -- 6.1 INTRODUCTION -- 6.2 ASSAY -- 6.3 IMPURITIES -- References -- Chapter 7 - Residual solvents -- 7.1 INTRODUCTION -- 7.2 CLASSES OF RESIDUAL SOLVENTS.

7.3 ANALYTICAL METHODS AND THEIR VALIDATION -- References -- Chapter 8 - Validation of procedures for elemental impurities -- 8.1 INTRODUCTION -- 8.2 ELEMENTAL IMPURITIES -- 8.3 VALIDATION PRINCIPLES (TRADITIONAL AND STANDARDIZED) -- 8.4 CONCLUSIONS -- References -- Part 3 - Specific Tests: Drug Substance -- Chapter 9 - Solid-state characterization -- 9.1 INTRODUCTION -- 9.2 VALIDATION -- 9.3 SAMPLE PREPARATION -- 9.4 FEASIBILITY TESTING -- 9.5 IDENTIFICATION TESTS -- 9.6 LIMIT TESTS -- 9.7 QUANTITATIVE METHODS -- 9.8 SYSTEM SUITABILITY AND GOODNESS-OF-FIT -- 9.9 CONCLUSIONS -- References -- Chapter 10 - Chiral methods -- 10.1 INTRODUCTION -- 10.2 IMPLEMENTATION OF HEALTH AUTHORITY GUIDELINES TO CHIRAL DRUG DEVELOPMENT -- 10.3 CHIRAL LC -- 10.4 OTHER CHIRAL SEPARATION METHODS -- 10.5 NONSEPARATION TECHNIQUES -- 10.6 CHIRAL METHOD VALIDATION -- 10.7 CONCLUSIONS -- Acknowledgments -- References -- Chapter 11 - Water determination -- 11.1 INTRODUCTION -- 11.2 LOSS ON DRYING (LOD) -- 11.3 KARL FISCHER TITRATION (KFT) -- 11.4 GAS CHROMATOGRAPHIC METHODS -- 11.5 NEAR-INFRARED SPECTROSCOPY -- References -- Part 4 - Specific Tests: Drug Product -- Chapter 12 - Dissolution -- 12.1 INTRODUCTION -- 12.2 THE DISSOLUTION TEST -- 12.3 VALIDATION AND METHOD DEVELOPMENT ASPECTS -- 12.4 ANALYTICAL VALIDATION -- 12.5 SOURCES OF ERROR IN DISSOLUTION TESTING -- 12.6 PERFORMANCE VERIFICATION OF DISSOLUTION EQUIPMENT -- 12.7 REGULATORY GUIDELINES -- References -- Chapter 13 - Extractables and leachables -- 13.1 INTRODUCTION -- 13.2 OVERVIEW OF THE STUDY DESIGN -- 13.3 EXTRACTION STUDY -- 13.4 EXTRACTABLE ANALYSIS -- 13.5 LEACHABLE STUDY -- 13.6 IMPACT OF LEACHABLES IN THE DRUG PRODUCT ABOVE THE AET -- 13.7 COMBINATION MEDICAL DEVICES -- 13.8 CONCLUSIONS -- Acknowledgments -- References -- Chapter 14 - Pharmacopeial methods and tests -- 14.1 INTRODUCTION.

14.2 LEGAL STATUS -- 14.3 REQUIREMENTS FOR INCLUSION -- 14.4 PROCESS FOR REVISION -- 14.5 TYPES OF TESTS -- 14.6 COMPENDIAL REFERENCE STANDARDS -- 14.7 HARMONIZATION -- References -- Part 6 - Microbial Methods -- Chapter 15 - Microbial methods -- 15.1 INTRODUCTION -- 15.2 MICROBIAL TESTING (PHASED APPROACH) -- 15.3 ALTERNATIVE RAPID MICROBIOLOGICAL METHODS -- 15.4 RAPID STERILITY TEST METHODS -- 15.5 RAPID BIOBURDEN METHODS -- 15.6 VALIDATION OF ALTERNATIVE METHODS -- 15.7 CONCLUSION -- References -- Part 7 - Biological Fluids -- Chapter 16 - Bioanalytical method validation and bioanalysis in regulated settings -- 16.1 INTRODUCTION-BRIEF HISTORY OF HARMONIZATION EFFORTS -- 16.2 GLP, GCP, AND REGULATED BIOANALYSIS -- 16.3 METHOD DEVELOPMENT AND INITIAL VALIDATION OF THE CHEMICAL METHOD -- 16.4 APPLICATION OF A VALIDATED METHOD TO ROUTINE DRUG ANALYSIS -- 16.5 BIOANALYTICAL REPORT -- 16.6 VALIDATION, PARTIAL VALIDATION, AND CROSSVALIDATION -- 16.7 BIOANALYTICAL METHOD VALIDATION-OTHER PARAMETERS AND ISSUES -- 16.8 EMERGING TECHNOLOGIES IN BIOANALYSIS -- 16.9 CONCLUSIONS -- Acknowledgments -- References -- Index.