Handbook of Analytical Validation

Introduction to Analytical Method ValidationIntroduction

The Drug Development Process

FDA Hierarchy and Organization

The International Conference on Harmonization

AMV Guidance

The Validation Process

Training

Conclusion

Analytical Instrument Qualification

Introduction

Components of Data Quality

The AIQ Process

Roles and Responsibilities

Software Validation and Change Control

AIQ Documentation

Instrument Categories

Conclusion

HPLC Method Development and Optimization with Validation in Mind

Introduction

HPLC Method Development Approaches

Method Goals

HPLC Method Development Instrumentation

Method Optimization

Summary

Method Validation Basics

Introduction

Method Validation Guidelines

Terms and Definitions

Validation According to Method Type

Documentation

Summary

Robustness and System Suitability

Introduction

Robustness Studies for Method Validation

Robustness Study Experimental Design

Analyzing the Results

Documentation and Reporting

System Suitability Tests

System Suitability Standards

System Suitability Protocol

Method Adjustments to Meet System Suitability Requirements

Conclusion

Setting Specifications and Investigating Out-of-Specification Results

Introduction

Guidance for Setting Specifications

General Concepts for Developing and Setting Specifications

Universal Tests/Criteria

Specific Tests/Criteria: New Drug Substances

Specific Tests/Criteria: New Solid Oral Drug Products

Specific Tests/Criteria: New Oral Liquid Drug Products

Specific Tests/Criteria: Parenteral Drug Products

Decision Trees

OOS Background

Preventing OOS Results

Identifying and Assessing OOS Test Results

Investigating OOS Test Results

Concluding the OOS Investigation

Validation by Type of Method

Introduction

Validation of Impurity Methods

Developing and Validating SIMs

Developing and Validating Dissolution Procedures

Bioanalytical Methods

Validating Peptide Mapping Methods

Cleaning Method Validation

Analytical Method Transfer

Introduction

Terms, Definitions, and Responsibilities

Analytical Method Transfer Options

Documentation of Results: The AMT Report

Potential AMT Pitfalls

Implementing New Technology in a Regulated Environment

Introduction

Changes to an Approved Method

What Constitutes a Change to a Method?

Implement an Existing Standard Method

Implement an Existing Standard Method with Adjustments

Implement an Existing Standard Method with Changes

Glossary of Terms Related to Chromatographic Method Validation

Appendix 1 Example Method Validation Protocol