Method Validation in Pharmaceutical Analysis A Guide to Best Practice

The second edition of the best-selling practical guide to pharmaceutical analytics has been completely redesigned to take account of the Quality by Design (QbD) concept that has become the gold standard in pharmaceutical manufacturing. Two real-life case studies are included.This second edition of a global bestseller has been completely redesigned and extensively rewritten to take into account the new Quality by Design (QbD) and lifecycle concepts in pharmaceutical manufacturing.As in the first edition, the fundamental requirements for analytical method validation are covered, but the second edition describes how these are applied systematically throughout the entire analytical lifecycle. QbD principles require adoption of a systematic approach to development and validation that begin with predefined objectives. For analytical methods these predefined objectives are established as an Analytical Target Profile (ATP). The book chapters are aligned with recently introduced standards and guidelines for manufacturing processes validation and follow the three stages of the analytical lifecycle: Method Design, Method Performance Qualification, and Continued Method Performance Verification. Case studies and examples from the pharmaceutical industry illustrate the concepts and guidelines presented, and the standards and regulations from the US (FDA), European (EMA) and global (ICH) regulatory authorities are considered throughout.The undisputed gold standard in the field.

ForewordANALYTICAL VALIDATION WITHIN THE PHARMACEUTICAL LIFECYCLEDevelopment of Process and Analytical Validation ConceptsAlignment between Process and Analytics: Three-Stage ApproachPredefined Objectives: Analytical Target ProfileAnalytical Life CycleANALYTICAL INSTRUMENT QUALIFICATIONAnalytical Instrument and System QualificationEfficient and Economic HPLC Performance QualificationESTABLISHMENT OF MEASUREMENT REQUIREMENTS - ANALYTICAL TARGET PROFILE AND DECISION RULESIntroductionDefining the Fitness for Intended UseDecision RulesOverview of Process to Develop Requirements for Procedure PerformanceDecision Rules and ComplianceCalculating Target Measurement UncertaintyTypes of Decision RulesTarget Measurement Uncertainty in the Analytical Target ProfileBias and Uncertainty in a ProcedureATP and Key Performance IndicatorsMeasurement UncertaintyExampleConclusionESTABLISHMENT OF MEASUREMENT REQUIREMENTS - PERFORMANCE-BASED SPECIFICATIONIntroductionIntended PurposeIdentificationAssayImpuritiesLimit TestsQuantitative TestsSummaryMETHOD PERFORMANCE CHARACTERISTICSIntroductionPrecisionAccuracy and RangeSpecificityLinearityDetection and Quantitation LimitGlossaryMETHOD DESIGN AND UNDERSTANDINGIntroductionAnalytical Quality by Design and Robustness InvestigationsCase Study: Robustness InvestigationsSystem Suitability TestsMETHOD PERFORMANCE QUALIFICATIONIntroductionCase Study: Qualification of an HPLCMethod for Identity, Assay, and Degradation ProductsDesign and Qualification of a Delivered Dose Uniformity Procedure for a Pressurized Metered Dose InhalerImplementation of Compendial/Pharmacopeia Test ProceduresTransfer of Analytical ProceduresCONTINUED METHOD PERFORMANCE VERIFICATIONIntroductionRoutine MonitoringInvestigating and Addressing Aberrant DataContinual ImprovementIndex