FDA方法验证

CONTAINSNON-BINDINGRECOMMENDATIONS#135GuidanceforIndustryValidationofAnalyticalProceduresforTypeCMedicatedFeedsThisguidancediscussescharacteristicsthatmaybeconsideredduringthevalidationofnon-microbiologicalanalyticalproceduresfortheanalysisofdrugsinTypeCmedicatedfeedsincludedaspartoforiginalandsupplementalnewanimaldrugapplications(NADAs)andabbreviatednewanimaldrugapplications(ANADAs)forTypeAMedicatedArticlessubmittedtotheFoodandDrugAdministration(FDA).Itprovidesguidanceandrecommendationsonconsideringvariousvalidationcharacteristicsforeachanalyticalprocedureusedinmedicatedfeedassaysandindicatesthedatathatmaybeincludedintheapplications.CommentsandsuggestionsregardingthisguidanceshouldbesenttotheDivisionofDocketsManagement(HFA-305),FoodandDrugAdministration,5630FishersLane,Room1061,Rockville,MD20852.AllcommentsshouldbeidentifiedwiththeDocketNo.2004D-0146.CommentsmayalsobesubmittedelectronicallyontheInternetat(HFV-141),FoodandDrugAdministration,7500StandishPlace,Rockville,MD20855,301-827-6964,E-mail:[e-mail]idancedocumentmayberequestedfromtheCommunicationsStaff(HFV-12),CenterforVeterinaryMedicine,FoodandDrugAdministration,7519StandishPlace,Rockville,MD20855,andmaybeviewedontheInternetat(expires12/31/07)and0910-0154(expires12/31/07).Thisguidancecontainsnonewcollectionsofinformation.___________________________________________________________________U.S.DepartmentofHealthandHumanServicesFoodandDrugAdministrationCenterforVeterinaryMedicineNovember7,2005CONTAINSNON-BINDINGRECOMMENDATIONS2TABLEOFCONTENTSPageNo.Introduction4Discussion51.Specificity62.Linearity73.Range74.Accuracy85.Precision85.1.Repeatability85.2.IntermediatePrecision85.3.Reproducibility95.4.ProofofPerformance96.LimitofDetection96.1.BasedonVisualEvaluation96.2.BasedonSignal-to-Noise96.3.BasedontheStandardDeviationoftheResponseandtheSlope106.3.1.BasedontheStandardDeviationoftheBlank106.3.2.BasedontheCalibrationCurve107.LimitofQuantitation107.1.BasedonVisualEvaluation107.2.BasedonSignal-to-NoiseApproach11CONTAINSNON-BINDINGRECOMMENDATIONS37.3.BasedontheStandardDeviationoftheResponseandtheSlope117.3.1.BasedontheStandardDeviationoftheBlank117.3.2.BasedontheCalibrationCurve118.Robustness/Ruggedness119.SystemSuitabilityTesting1210.RecommendedData12Glossary15CONTAINSNON-BINDINGRECOMMENDATIONS4GuidanceforIndustryValidationofAnalyticalProceduresforTypeCMedicatedFeeds1INTRODUCTIONThepurposeofthisguidanceistoproviderecommendationsonhowtoconsiderthevariousvalidationcharacteristicsforeachanalyticalprocedureusedinmedicatedfeedassays.Thisguidanceiswrittenprimarilyforchromatographicmethods;however,theguidancedoesnotlimittheanalyticaltechniquetochromatographicprocedures,asothertechniquesmaybeappropriate.Insomecases(forexample,demonstrationofspecificity),theoverallcapabilitiesofanumberofanalyticalproceduresincombinationmaybeinvestigatedinordertoensurethequalityofthemedicatedfeed.Section512(b)oftheFederalFood,Drug,andCosmeticAct(21U.S.C.§360b)establishestherequirementsfornewanimaldrugapproval.21C.F.R.§514.1specifiestheinformationrequiredtobesubmittedaspartoftheapplicationandtheproperformforthesubmission.Section514.1(b)(5)(vii)requiresanapplicanttodescribeanalyticalproceduresthatshouldbecapableofdeterminingtheactivecomponent(s)withinareasonabledegreeofaccuracyandofassuringtheidentityofsuchcomponents.Section514.1(b)(5)(vii)(a)statesthatadescriptionofpracticable1ThisguidancehasbeenpreparedbytheOfficeofNewAnimalDrugEvaluationintheCenterforVeterinaryMedicineattheFoodandDrugAdministration.Thisguidancerepresentstheagency’scurrentthinkingonthistopic.ItdoesnotcreateorconferanyrightsfororonanypersonanddoesnotoperatetobindFDAorthepublic.Youcanuseanalternativeapproachiftheapproachsatisfiestherequirementsoftheapplicablestatute(s)andregulation(s).Ifyouwanttodiscussanalternativeapproach,contacttheFDAstaffresponsibleforimplementingthisguidance.IfyoucannotidentifytheappropriateFDAstaff,calltheappropriatenumberlistedonthetitlepageofthisguidance.CONTAINSNON-BINDINGRECOMMENDATIONS5methodsofanalysisofadequatesensitivitytodeterminetheamountofthenewanimaldruginthefinaldosageformshouldbeincluded.FDA’sguidancedocuments,includingthisguidance,donotestablishlegallyenforceableresponsibilities.Instead,guidancesdescribetheAgency’scurrentthinkingonatopicandshouldbeviewedonlyasrecommendations,unlessspecificregulatoryorstatutoryrequirementsarecited.Theuseoftheword“should”inAgencyguidancesmeansthatsomethingissuggestedorrecommended,butnotrequired.DISCUSSIONTheobjectiveoftheanalyticalprocedureshouldbeclearlyunderstoodsincethiswillgovernthevalidationcharacteristicsthatareevaluated.Typicalvalidationcharacteristicsthatmaybeconsideredarelistedbelow:-Specif