Validation of analytical methods

cGMPGCPISO17025PIC/SGxPFDALOD/LOQOECDQA/QCAPIEPSOPUSP1225/1226ICHQ2(R1)ValidationofAnalyticalMethodsValidationofAnalyticalMethods©Copyright2010AgilentTechnologiesPrintedinGermany,March1,2010PublicationNumber5990-5140EN:Validationvs.Verification...................41.3ElementsofDataQualityinLaboratories..................42.RegulationsandQualityStandards.......................72.1UnitedStatesFoodandDrugAdministration(FDA).........82.2PharmaceuticalInspectionCooperationScheme(PIC/S)andEurope.........................................92.3InternationalConferenceforHarmonization(ICH)..........102.4UnitesStatesPharmacopeia(USP).....................112.5ISO/IEC17025.....................................113.ParametersandTestsforMethodValidation..............133.1Specificity/Selectivity................................153.2Precision..........................................183.3AccuracyandRecovery..............................193.4LinearityandCalibrationCurve........................203.5Range............................................223.6LimitofDetection...................................233.7LimitofQuantitation.................................243.8Ruggedness.......................................263.9Robustness........................................263.10Stability.........................................26ContentsI4.MethodValidationProcess.............................294.1LifeCycleConcept..................................304.2ValidationPlanning..................................314.3ScopeandMethodSpecifications......................324.4SelectingValidationParametersandLimits...............334.5TestingforPerformanceCharacteristics:PreparationandExecution............................364.6DevelopingaQualityControlPlanforRoutineAnalysis.....384.7ValidationReportandotherDocumentation..............395.MethodAdjustments,ChangesRevalidation,andVerificationofStandardandCompendialMethods....415.1MethodAdjustments................................425.2Revalidation.......................................465.3VerificationofStandardandCompendialMethods.........466.TransferofAnalyticalMethods.........................516.1TransferProcedures.................................526.2StepsforMethodTransfer............................537.ValidationofBioanalyticalMethods.....................557.1ValidationGuidelinesfromConferencesandFDA..........567.2ValidationParameters...............................587.3QualityControlinBioanalyticalRoutineAnalysis...........60References............................................61Glossary...............................................65IIThisprimerisintendedtoguidemanagersandanalystsfrom(bio)pharma-ceutical,food,chemical,environmentalandotherregulatedlaboratoriesthroughallaspectsofanalyticalmethodsvalidation.Qualitymanagersandstaffaswellasregulatoryaffairsprofessionalswillalsobenefitthroughextensivediscussionsofrelevantregulations,qualitystandardsandguidelines.Theprimerwillgivestrategiesandspecificrecommendationsforthevalidationofnewmethodsthataredevelopedinternallyaswellasfortheverificationofcompendialandstandardmethods.Inlessthanonedayreaderswillget:•Anoverviewofregulatoryandqualitystandardrequirements•Aliteratureoverview•Strategiesforimplementation•Informationontestparameters,acceptancecriteriaandtestconditions•Recommendationsforspecialapplications,suchasvalidationofbioanalyticalmethods,verificationofcompendialmethodsandtransferofanalyticalmethodsTheconceptsandideasexpressedinthisprimeraremyownanddonotnecessarilyreflectofficialAgilentorLabcompliancepolicies.SometextinformationandfiguresinthisprimerhavebeentakenfromDr.LudwigHuber’sreferencebookwithpermissionfromthepublisherINFORMAHEALTHCARE,NewYork.•L.Huber,ValidationandQualificationinAnalyticalLaboratories,Interpharm,InformaHealthcare,NewYork,USA,2007Copyrightofthetextandfiguresresideswiththepublisher.Regulationsandqualitystandardsaredynamic.Theyareupdatedeveryfewyears.Implementationguidelines,asdevelopedbyregulatorytaskandindustrytaskforces,arepublishedmorefrequentlysincestate-of-thearttodaymaynotbeconsideredassuchinthefuture.PrefaceIIIAtimelyupdateofallinformationisimportantandonlypossibleusingon-lineinformationtools,suchastheInternet.Therefore,Irecommendthefollowingwebsiteswithregularupdatesrelatedtoqualitystandardsinlaboratories:://@labcompliance.comIVChapter1IntroductionIntroductionT