Method Validation in Pharmaceutical Analysis: A Guide to Best Practice

437 Pages·2014·4.37 MB·English

by  Joachim Ermer

Editedby
JoachimErmerandPhilNethercote
MethodValidationinPharmaceutical
Analysis
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EditedbyJoachimErmerandPhilNethercote
Method Validation in Pharmaceutical
Analysis
AGuidetoBestPractice
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V
Contents
Foreword XIII
ListofContributors XV
1 AnalyticalValidationwithinthePharmaceuticalLifecycle 1
PhilNethercoteandJoachimErmer
1.1 DevelopmentofProcessandAnalyticalValidationConcepts 1
1.2 AlignmentbetweenProcessandAnalytics:Three-StageApproach 4
1.3 PredefinedObjectives:AnalyticalTargetProfile 5
1.4 AnalyticalLifeCycle 8
References 9
2 AnalyticalInstrumentQualification 11
2.1 AnalyticalInstrumentandSystemQualification 11
ChristopherBurgessandR.D.McDowall
2.1.1 DataQualityandIntegrityinaGMPEnvironment 11
2.1.1.1 CriteriaforQualityData 11
2.1.1.2 RegulatoryRationaleforQualifiedAnalyticalInstruments 12
2.1.2 USPGeneralChapter<1058> 12
2.1.2.1 DataQualityTriangle 14
2.1.2.2 AnalyticalInstrumentQualificationLifeCycle:theFourQs
Model 14
2.1.2.3 Risk-BasedClassificationofApparatus,Instruments,and
Systems 15
2.1.2.4 RolesandResponsibilitiesforAIQ 17
2.1.2.5 SoftwareValidationforGroupBandCSystems 18
2.1.3 Enhancementof<1058>andHarmonizationofaRisk-Based
ApproachtoInstrumentsandSystemswithGAMPLaboratoryGPG
SecondEdition 18
2.1.3.1 IncreasedGranularityofUSP<1058>Groups 18
2.1.3.2 ClarificationofAIQTerminology 19
2.1.3.3 AContinuumofAnalyticalApparatus,Instruments,and
Systems 19
VI Contents
2.1.3.4 MappingUSP<1058>InstrumentGroupstoGAMPSoftware
Categories 20
2.1.3.5 EnhancedDataQualityTriangle 20
2.1.4 Risk-BasedApproachestoAnalyticalInstrumentandSystem
Qualification 20
2.1.4.1 Expanded<1058>InstrumentandSystemCategories 23
2.2 EfficientandEconomicHPLCPerformanceQualification 25
HermannWätzig
2.2.1 Introduction 25
2.2.1.1 TheImportanceofAnalyticalInstrumentQualification 25
2.2.1.2 TermsandDefinitions 25
2.2.1.3 ContinuousPerformanceQualification:MorebyLess 27
2.2.2 DevelopmentoftheRevisedOQ/PQParametersList 27
2.2.3 TransferofModularParametersintotheHolisticApproach 29
2.2.3.1 Autosampler 29
2.2.3.2 SolventDeliverySystem 29
2.2.3.3 Detector 30
2.2.4 OQ/PQDatainComparisonwithSSTData 32
2.2.5 ControlCharts 33
2.2.6 GeneralProcedureforContinuousPQ 34
2.2.7 ConcludingRemarks 36
Acknowledgment 37
Abbreviations 37
References 38
3 EstablishmentofMeasurementRequirements–AnalyticalTarget
ProfileandDecisionRules 41
MaryLeeJaneWeitzel
3.1 Introduction 41
3.2 DefiningtheFitnessforIntendedUse 42
3.3 DecisionRules 42
3.4 OverviewofProcesstoDevelopRequirementsforProcedure
Performance 43
3.5 DecisionRulesandCompliance 43
3.6 CalculatingTargetMeasurementUncertainty 45
3.6.1 CoverageFactor,k,andDataDistributions 46
3.7 TypesofDecisionRules 47
3.7.1 DecisionRulesThatUseGuardBands 48
3.8 TargetMeasurementUncertaintyintheAnalyticalTargetProfile 49
3.8.1 CostofAnalysis 49
3.9 BiasandUncertaintyinaProcedure 50
3.10 ATPandKeyPerformanceIndicators 51
3.11 MeasurementUncertainty 51
3.11.1 WhatUncertaintyIs 51
3.11.2 ReportingMeasurementUncertainty 52
Contents VII
3.11.3 HowUncertaintyisEstimated 54
3.11.4 UncertaintyContainsAllSourcesofRandomVariability 55
3.12 Example 56
3.13 Conclusion 57
References 58
4 EstablishmentofMeasurementRequirements–Performance-Based
Specifications 59
ToddL.Cecil
4.1 Introduction 59
4.2 IntendedPurpose 60
4.3 Identification 60
4.4 Assay 62
4.4.1 Precision 62
4.4.2 Accuracy 63
4.4.3 PrecisionandAccuracy 64
4.4.3.1 RelationshipbetweenAccuracyandPrecision 64
4.4.4 Specificity 65
4.4.4.1 ChromatographicProcedures 65
4.4.4.2 Non-chromatographicProcedures 66
4.4.5 LinearityandRange 67
4.4.5.1 Linearity 67
4.4.5.2 Range 67
4.5 Impurities 68
4.6 LimitTests 69
4.6.1 LimitofDetection 69
4.6.2 Precision 70
4.6.3 Specificity 70
4.7 QuantitativeTests 70
4.7.1 Accuracy 70
4.7.2 Precision 71
4.7.3 SpecificityandRange 71
4.8 Summary 71
References 71
5 MethodPerformanceCharacteristics 73
JoachimErmer
5.1 Introduction 73
5.2 Precision 74
5.2.1 DistributionofData 74
5.2.1.1 TheNormalDistributionanditsParameters 74
5.2.1.2 RobustParameter 84
5.2.2 PrecisionLevels 84
5.2.2.1 SystemorInstrumentPrecision 85
5.2.2.2 Repeatability 86
VIII Contents
5.2.2.3 IntermediatePrecisionandReproducibility 86
5.2.3 CalculationofPrecisionsandVariances 89
5.2.3.1 AnalysisofVariances(ANOVA) 90
5.2.3.2 CalculationofPrecisionfromLinearRegression 92
5.2.4 ConcentrationDependencyofPrecision 93
5.2.5 PrecisionAcceptanceCriteria 95
5.2.5.1 PrecisionoftheReportableResult 95
5.2.5.2 OptimizationoftheCalibrationFormat 97
5.2.5.3 AcceptablePrecisionforAssay 101
5.2.5.4 AcceptablePrecisionforImpuritiesandMinorComponents 105
5.2.6 PrecisionsBenchmarks 107
5.2.6.1 PrecisionsforLCAssay 108
5.2.7 SourcestoObtainandSupplementPrecisions 116
5.2.7.1 PrecisionsfromStability 117
5.2.8 PrecisionHighlights 119
5.3 AccuracyandRange 119
5.3.1 DrugSubstance 122
5.3.1.1 SignificanceTests 122
5.3.1.2 EquivalenceTests 124
5.3.1.3 DirectComparison 125
5.3.1.4 ComparisonExamples 125
5.3.2 DrugProduct 126
5.3.2.1 PercentageRecovery 127
5.3.2.2 RecoveryFunction 128
5.3.2.3 StandardAddition 128
5.3.2.4 AccuracyofDrugProductbyComparison 129
5.3.3 Impurities/Degradants 129
5.3.3.1 RecoveryofSpikedImpurities 129
5.3.3.2 AccuracyoftheIntegrationMode 130
5.3.3.3 ResponseFactors 131
5.3.4 AcceptanceCriteria(ATPRequirements) 132
5.3.4.1 CanthisTheoreticallyObtainedRelationshipbeSupportedby
ExperimentalResults? 135
5.3.5 JointEvaluationofAccuracyandPrecision 136
5.3.6 AccuracyHighlights 137
5.4 Specificity 137
5.4.1 DemonstrationofSpecificitybyAccuracy 140
5.4.2 ChromatographicResolution 140
5.4.3 PeakPurity(Co-elution) 141
5.4.3.1 Rechromatography 141
5.4.3.2 DiodeArrayDetection 142
5.4.3.3 LC-MS 143
5.4.4 SpecificityHighlights 145
5.5 Linearity 145
5.5.1 UnweightedLinearRegression 147