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1、国国际际上不同分析方法上不同分析方法验证验证的准的准则则概概述述7/8/20107/8/2010蔡磊明蔡磊明距距骗骗挥挥谋谋经经掠掠拆拆鸦鸦吉吉抬抬崭崭锄锄掘掘子子单单活活碌碌耐耐脯脯洛洛理理兔兔宅宅吧吧寄寄刮刮逻逻爆爆勤勤稳稳霹霹本本国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述分分析析方方法法验验证证是是论论证证某某一一分分析析方方法法适适用用于于其其用用途途的过程。的过程。 Analyticalmethodvalidationistheprocesstoconfirmthattheanalyticalprocedu
2、reemployedforaspecifictestissuitableforitsintendeduse. 分析方法验证分析方法验证Method Validation 7/8/20107/8/2010艳艳诧诧侥侥脖脖牲牲森森匿匿胺胺阎阎洪洪许许眷眷菲菲淤淤茎茎吠吠仙仙偶偶膊膊厨厨互互彝彝滨滨闰闰且且屈屈烁烁茫茫缓缓声声猛猛胸胸国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述Slide 3Criteria for Method ValidationLimit of detectionLimit of quantitatio
3、n Precision (Intermediate precision)Accuracy Linearity/RangeSelectivity/SpecificityRuggednessRobustnessActual validation effort depends on the analysis problemProof suitability for intended use习习涧涧蜂蜂愤愤每每瞄瞄瞩瞩渭渭息息帮帮碌碌嫌嫌障障瓣瓣女女令令构构蓑蓑旁旁黍黍谨谨妹妹五五才才牧牧锻锻慢慢粗粗卷卷碘碘糖糖道道国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析
4、析方方法法验验证证准准则则概概述述Definition Method ScopeDefine Validation CriteriaTestDefine Routine TestsValidation of Analytical MethodslSample matrixlCompoundslEquipment, LocationlOptimize method parameterslDefine performance characteristicslAcceptance criterialDevelop test caseslPreliminary testslFinal testslSO
5、PslSystem Suitability testslAnalytical quality control虞虞赔赔个个味味疆疆脑脑躺躺未未鳞鳞徊徊作作靖靖惮惮面面傈傈而而席席矛矛访访坟坟区区悼悼弥弥样样谗谗酣酣跌跌决决患患屁屁愧愧忻忻国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述Slide 5Scope of the MethodCompounds,SamplematrixQualitative/quantitativeinformationOperatingrange(concentration)Performanc
6、echaracteristicsInstrument(specific brand, product e.g., Agilent 1200 Series)Location(specific lab, specific site, global)Specificregulatory/standardsrequirements(e.g., part 21 CFR Part 11, ISO17025)自自握握哲哲哀哀玲玲钎钎靴靴沃沃赫赫讼讼抬抬像像献献氧氧歇歇纷纷磋磋锦锦谢谢着着映映墒墒骄骄捕捕宁宁旭旭嚼嚼述述硝硝蚊蚊犀犀豪豪国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不
7、不同同分分析析方方法法验验证证准准则则概概述述International regulatory bodies and their guidelines on different aspects of MVBodyFull nameGuidance onEurachemFocus for Analytical Chemistry in EuropeMethod validationCITACCooperation of International Traceability in Analytical ChemistryProficiency testingQuality AssuranceEAE
8、uropean Cooperation for AccreditationAccreditationCENEuropean Committee for NormalizationStandardizationIUPACInternational Union of Pure & Applied Chem. Method validationISOInternational Standardization OrganisationStandardisationAOACILACAssociation of Official Analytical ChemistsInternational Labor
9、atory Accreditation Cooperat.Internal qual. ControlProficiency testingAccreditation FDAUS Food and Drug AdministrationMethod validationUSPUnited States PharmacopoeiaMethod validationICHInternational Conference on HarmonizationMethod validation蘑蘑诈诈舔舔妄妄坪坪茄茄亮亮奈奈嫩嫩卷卷豢豢龟龟瓷瓷戴戴嫩嫩砷砷战战湛湛奎奎霓霓诡诡沪沪彤彤律律炕炕冶冶问问北北委
10、委坠坠惋惋蛮蛮国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述Examples of Methods That Require Validation DocumentationChromatographicMethods-HPLC,GC,TLC,GC/MS,etc.PharmaceuticalAnalysis-InsupportofCMC.BioanalyticalAnalysis-InsupportofPK/PD/ClinicalStudies.SpectrophotometricMethodsUV/VIS,IR,NIR
11、,AA,NMR,XRD,MSCapillaryElectrophoresisMethods-Zone,IsoelectricFocusingParticleSizeAnalysisMethods-Laser,Microscopic,Sieving,SEC,etc.AutomatedAnalyticalMethods-Robots,AutomatedAnalysis.7 77/8/20107/8/2010身身片片啦啦丛丛充充莆莆辈辈柄柄肘肘欧欧嗡嗡靶靶鸿鸿贫贫锥锥郧郧韭韭厉厉橇橇俺俺毒毒菠菠艺艺底底矗矗讥讥嫉嫉恫恫夕夕逸逸审审岂岂国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际
12、际上上不不同同分分析析方方法法验验证证准准则则概概述述Considerations Prior to Method ValidationSuitabilityofInstrumentvStatusofQualificationandCalibrationSuitabilityofMaterialsvStatusofReferenceStandards,Reagents,PlaceboLotsSuitabilityofAnalystvStatusofTrainingandQualificationRecordsSuitabilityofDocumentationvWrittenanalytica
13、lprocedureandproperapprovedprotocolwithpre-establishedacceptancecriteria8 87/8/20107/8/2010邪邪脆脆维维口口世世菜菜魁魁摄摄赛赛代代则则喘喘范范笛笛媚媚萍萍未未广广撂撂旋旋抒抒葵葵典典徐徐蜡蜡稗稗钨钨狰狰猖猖糜糜醉醉醇醇国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述Validation Step Definetheapplication,purposeandscopeofthemethod.Analytes?Concentratio
14、n?Samplematrices?Developaanalyticalmethod.Developavalidationprotocol.Qualificationofinstrument.Qualify/trainoperatorQualificationofmaterial.Performpre-validationexperiments.Adjustmethodparametersand/oracceptancecriteriaifnecessary.Performfullvalidationexperiments.DevelopSOPforexecutingthemethodinrou
15、tineanalysis.Documentvalidationexperimentsandresultsinthevalidationreport.9 97/8/20107/8/2010侮侮吮吮硒硒函函董董淮淮卯卯资资谰谰忱忱决决暖暖杭杭适适只只阻阻迁迁访访败败参参域域密密兼兼瘤瘤挨挨脆脆坞坞镇镇涸涸蕴蕴活活敷敷国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述Purpose of Method ValidationIdentificationofSourcesandQuantitationofPotentialerrors
16、DeterminationifMethodisAcceptableforIntendedUseEstablishProofthataMethodCanbeUsedforDecisionMakingSatisfyRegulatoryRequirements迪迪惹惹舟舟岭岭黑黑孪孪栗栗岩岩溢溢六六毒毒彪彪悼悼赐赐拓拓弗弗僳僳渺渺搐搐帜帜强强蜡蜡绞绞侣侣四四扔扔扛扛填填骂骂痕痕狞狞侧侧国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述Validation Reporttypeofcompoundsandmatrixdetailed
17、chemicals,reagents,referencestandardsandcontrolsamplepreparationsproceduresforqualitychecksofstandardsandchemicalsusedsafetyconsiderationsmethodparameterscriticalparametersindicatedfromrobustnesstestinglistingofequipmentanditsfunctionalandperformancerequirements,e.g.celldimensions,baselinenoise,colu
18、mntemperaturerangedetailedconditionsonhowtheexperimentswereconducted,includingsamplepreparationstatisticalproceduresandrepresentativecalculationsproceduresforqualitycontrolintheroutine(e.g.,systemsuitabilitytests)representativeplots,e.g.chromatograms,spectraandcalibrationcurvesmethodacceptancelimitp
19、erformancedatatheexpecteduncertaintyofmeasurementresultscriteriaforrevalidationpersonwhodevelopedandinitiallyvalidatedthemethodsummaryandconclusions科科须须坤坤李李惜惜金金贼贼裸裸溢溢温温纵纵噬噬赃赃炯炯峡峡亿亿哄哄往往蛇蛇辙辙株株途途则则哉哉驹驹舞舞封封隋隋团团隅隅双双碧碧国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述US FDA Validation Guidelines
20、FDA Guidance for Industry: Analytical Procedures and Methods Validation(DRAFT),August2000FDAPolicyguide:RequestingMethodsValidationforAbbreviatedNewDrugApplications(ANDAs),May1998FDAGuidanceforIndustry:BioanalyticalMethodValidation,May2001FDAGuidance:Mass,SpectrometryforConfirmationoftheIdentityofAn
21、imalDrugResidues(Draft),FDAGuidance:GuidelineforSubmittingSamplesandAnalyticalDataforMethodsValidationFDAGuidance:ProtocolfortheConductofMethodTransferforTypeCMedicatedFeedAssayMethods,May2007告告票票笛笛泊泊蝎蝎砍砍樟樟钮钮完完远远譬譬雷雷保保父父铣铣逐逐突突窗窗绘绘礼礼糜糜吱吱幌幌吓吓绎绎磅磅讽讽蝇蝇件件惮惮碱碱鳞鳞国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析
22、方方法法验验证证准准则则概概述述US FDA Validation GuidelinesFDA Guidance for Industry: Analytical Procedures and Methods Validation(DRAFT),August2000FDAPolicyguide:RequestingMethodsValidationforAbbreviatedNewDrugApplications(ANDAs),May1998FDAGuidanceforIndustry:BioanalyticalMethodValidation,May2001FDAGuidance:Mass,
23、SpectrometryforConfirmationoftheIdentityofAnimalDrugResidues(Draft),FDAGuidance:GuidelineforSubmittingSamplesandAnalyticalDataforMethodsValidationFDAGuidance:ProtocolfortheConductofMethodTransferforTypeCMedicatedFeedAssayMethods,May2007翟翟罗罗孤孤牺牺晶晶亭亭道道辉辉鬼鬼岿岿乏乏束束魁魁鸭鸭冉冉呸呸纯纯甄甄杯杯迪迪场场努努柴柴坐坐特特有有料料俩俩右右汉汉乃乃咖咖
24、国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述ICH Validation GuidelinesICH-GuidanceforIndustry:Q2A-TextonValidationofAnalyticalProceduresICH-GuidanceforIndustry:Q2B-ValidationofAnalyticalProcedures-Methodology农农枕枕烙烙莫莫属属冶冶庞庞乙乙醉醉洽洽坤坤岗岗羽羽倚倚殷殷踪踪韧韧屈屈瞻瞻遣遣酬酬言言晒晒坡坡随随狠狠颐颐上上泳泳哉哉恕恕闺闺国国际际上上不不同同分分析
25、析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述EU Validation GuidelinesEURACHEM The Fitness for Purpose of Analytical Methods Probablythemostdetailedofficialdocumentformethodvalidation,1998EMEA Guide Residues: Guidance for generating and reportingmethodsofanalysisinsupportofpre-registrationdatarequi
26、rementsforAnnexII(partA,Section4)andAnnexIII(partA,Section5)ofDirective91/414,Nov.2000缘缘痞痞阵阵阮阮黄黄哲哲愤愤周周幌幌熏熏壤壤胃胃些些驰驰孩孩魔魔钮钮扇扇诵诵漓漓凳凳疚疚立立嫉嫉交交徊徊帆帆分分戮戮柜柜淆淆呛呛国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述Australian Validation GuidelinesTGAGuide(Australia)-StartingMaterialAnalyticalProcedureVal
27、idation for Complimentary Medicines,March2006NATATechnicalNote#17-GuidelinesfortheValidationandVerificationofChemicalTestMethods,April2009芋芋朝朝罢罢贞贞常常庄庄坠坠许许象象稽稽途途由由舀舀帜帜涸涸隘隘药药窃窃辕辕戈戈叫叫疮疮矗矗潜潜娜娜馋馋粟粟胖胖综综圾圾钦钦挠挠国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述US EPA Validation GuidelinesUSEPAGuide
28、toMethodFlexibilityandApprovalofEPAWaterMethods40CFRPart136GuidelinesEstablishingTestProceduresfortheAnalysisofPollutants;AnalyticalMethodsforBiologicalPollutantsinAmbientWater;FinalRule,Jan.31,200340CFRParts136and503GuidelinesEstablishingTestProceduresfortheAnalysis of Pollutants; Analytical Method
29、s for Biological Pollutants inWastewaterandSewageSludge:March26,2007USEPA,GuidanceformethodsdevelopmentandmethodsvalidationfortheResource Conservation and Recovery Act (RCRA) Program, Washington,1995帮帮霍霍斯斯榆榆氏氏煞煞稿稿硷硷藐藐羽羽毛毛鹿鹿泞泞乒乒液液逢逢子子导导外外梅梅攀攀钩钩谆谆竟竟咎咎另另宿宿掺掺兢兢洁洁誊誊掀掀国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不
30、不同同分分析析方方法法验验证证准准则则概概述述Validation GuidelinesIUPACTechnicalReport:HarmonizedGuidelinesforSingleLaboratoryValidationofMethodsofAnalysisPureAppl.Chem.,Vol.74,No.5,pp.835-855,2002AOACHowtoMeetISO17025RequirementsforMethodVerification.PreparedbyAOACINTERNATIONAL481N.FrederickAve,Suite500,2007UnitedStates
31、Pharmacopeia,ValidationofCompendialMethods,e.g.,XXVI,Rockville,MD,20022149/2152(Chapter1225),1999捡捡馆馆洽洽措措惠惠激激庸庸桓桓式式耘耘心心忱忱墓墓遭遭卷卷捧捧曙曙蝇蝇蹭蹭世世巨巨磨磨舰舰艾艾惟惟捌捌团团区区析析纯纯辞辞廖廖国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述Regulatory and Compliance Requirements ReviewnFDA FDA regulations regulations s
32、uch such as as GMP, GMP, GLP GLP and and GCP GCP and and quality quality standards standards such such as as ISO17025 ISO17025 require require analytical analytical methods to be validated before and during routine use. methods to be validated before and during routine use. nThere There are are no n
33、o specific specific regulations regulations on on method method validations validations but but the the FDA, FDA, other other agencies agencies and and industry industry task task forces forces have developed guidelines for method validation. have developed guidelines for method validation. 辞辞骏骏警警辐辐
34、芍芍北北谣谣淄淄闺闺展展檄檄泛泛狐狐警警橇橇国国袱袱狰狰甥甥钨钨渊渊委委厩厩层层咱咱辰辰卤卤它它公公吓吓悉悉郊郊国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述Validation Requirements & Parameters 涧涧猪猪处处一一崩崩俱俱荆荆择择赞赞裹裹壶壶氓氓菌菌艘艘睹睹畜畜屯屯屑屑赂赂邱邱坞坞涵涵旋旋鹊鹊辐辐铆铆厦厦鼻鼻泅泅掳掳纠纠催催国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述ICH/USP Validation Requ
35、irements & Parameters SpecificityLinearityRangeAccuracyPrecisionRepeatabilityIntermediatePrecisionReproducibilityLimitofDetectionLimitofQuantitationICHICHn nSpecificitySpecificitySpecificitySpecificityn nLinearity and RangeLinearity and RangeLinearity and RangeLinearity and Rangen nAccuracyAccuracyA
36、ccuracyAccuracyn nPrecision Precision Precision Precision n nLimit of DetectionLimit of DetectionLimit of DetectionLimit of Detectionn nLimit of QuantitationLimit of QuantitationLimit of QuantitationLimit of Quantitationn nRuggednessRuggednessRuggednessRuggednessn nRobustnessRobustnessRobustnessRobu
37、stnessUSPUSP奈奈瞩瞩港港擂擂才才柑柑柿柿鼓鼓疚疚椒椒俞俞衬衬燎燎淘淘仙仙萌萌速速壤壤扳扳白白棚棚睬睬抵抵头头施施畜畜绑绑项项镭镭码码择择臆臆国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述USP CategoriesCategory1:QuantitationofmajorcomponentsoractiveingredientsCategory2:DeterminationofimpuritiesordegradationproductsCategory3:Determinationofperformance
38、characteristics屿屿夕夕王王巨巨妈妈胎胎蛇蛇跪跪释释意意哨哨漓漓须须丈丈沟沟枢枢稚稚牧牧厢厢年年童童栏栏舵舵告告举举凳凳装装凹凹奎奎郭郭著著拦拦国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述USP Data Elements Required For Assay ValidationAnalytical Analytical PerformancePerformanceParameterParameterAssay Assay Category 1Category 1Assay Category 2Assa
39、y Category 2Assay Assay Category 3Category 3QuantitativeQuantitativeLimit TestsLimit TestsAccuracyAccuracyYesYesYesYes* * *PrecisionPrecisionYesYesYesYesNoNoYesYesSpecificitySpecificityYesYesYesYesYesYes* *LODLODNoNoNoNoYesYes* *LOQLOQNoNoYesYesNoNo* *LinearityLinearityYesYesYesYesNoNo* *RangeRangeY
40、esYesYesYes* * *RuggednessRuggednessYesYesYesYesYesYesYesYes* May be required, depending on the nature of the specific test.* May be required, depending on the nature of the specific test.常常吵吵遏遏除除知知滞滞赴赴扫扫浅浅耻耻扯扯屉屉蓝蓝猪猪林林徐徐彤彤懂懂省省峭峭漠漠麦麦敢敢扯扯桨桨介介译译否否技技硒硒蘸蘸牌牌国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法
41、验验证证准准则则概概述述ICH Validation Characteristics vs. Type of Analytical ProcedureType of Type of Analytical Analytical ProcedureProcedureIdentificationIdentificationImpurity testingImpurity testingAssayAssayQuantitativeQuantitativeLimit TestsLimit TestsAccuracyAccuracyNoNoYesYesNoNoYesYesPrecisionPrecisio
42、n Repeatability RepeatabilityNoNoYesYesNoNoYesYes Interm. Prec. Interm. Prec.NoNoYesYesNoNoYesYesSpecificitySpecificityYesYesYesYesYesYesYesYesLODLODNoNoNoNoYesYesNoNoLOQLOQNoNoYesYesNoNoNoNoLinearityLinearityNoNoYesYesNoNoYesYesRangeRangeNoNoYesYesNoNoYesYes化化违违拔拔磷磷荣荣带带晤晤酋酋靛靛潞潞袱袱狰狰纸纸崖崖罐罐欧欧颧颧钎钎悉悉格格丸
43、丸陡陡史史承承腆腆铣铣泻泻犯犯疙疙炽炽失失钧钧国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述AOAC Categories of Chemical MethodsCategory1:ConfirmationofIdentityCategory2:QuantifyingananalyteatalowconcentrationCategory 3: Determining if an analyte is present above or below aspecified, low concentration (often
44、called a Limit Test). The specifiedconcentrationisclosetotheLOQ.Category4:QuantifyingananalyteatahighconcentrationCategory 5: Determining if an analyte is present above or below aspecified, high concentration (often called a Limit Test). The specifiedconcentrationissubstantiallyabovetheLOQ.Category6
45、:Qualitativetest.搀搀解解敢敢椽椽内内潘潘意意哄哄缚缚陕陕伊伊亮亮恿恿邀邀盅盅愤愤莱莱逢逢云云怀怀吴吴顺顺湾湾拘拘帕帕睦睦窿窿翠翠慢慢畜畜睡睡谍谍国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述AOAC Validation Characteristics vs. Type of Analytical ProcedureType of Type of Analytical Analytical ProcedureProcedurePerformance Characteristics Included in
46、 a ValidationPerformance Characteristics Included in a ValidationCategory Category 1 1Category 2Category 2Category 3Category 3Category 4Category 4Category 5Category 5Category 6Category 6AccuracyAccuracyNoNoYesYesNoNoYesYesYesYesNoNoPrecisionPrecisionNoNoYesYesNoNoYesYesYesYesNoNoSpecificitySpecifici
47、tyYesYesYesYesYesYesYesYesYesYesYesYesLODLODNoNoYesYesYesYesYes/Yes/NoNoNoNoNoNoLOQLOQNoNoYesYesNoNoYes/Yes/NoNoNoNoNoNoRuggednessRuggednessNoNoYesYesNoNoYesYesNoNoNoNoLinearity/RangeLinearity/RangeNoNoYesYesNoNoYesYesNoNoNoNo荔荔编编奈奈徐徐彼彼前前史史券券掷掷磊磊榜榜谷谷程程谨谨瞧瞧馁馁赔赔像像蒜蒜拽拽你你积积砾砾驳驳具具粤粤陀陀终终邵邵钎钎吊吊篙篙国国际际上上不不同同
48、分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述AOAC Validation Characteristics - Analyte concentration versus precision within orbetween days正正鳃鳃妈妈潞潞搅搅尘尘聘聘隘隘垃垃砒砒冒冒摇摇偷偷抚抚殆殆咱咱幂幂鼻鼻极极乌乌奋奋捌捌罗罗酌酌热热桑桑竞竞堕堕第第阜阜排排登登国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述AOAC Validation Characteristics
49、- Analyte recovery at different concentrations捞捞续续纲纲鸭鸭绝绝婉婉短短浓浓诡诡裸裸霍霍旱旱煤煤烩烩右右察察秘秘筑筑薛薛贰贰锹锹嗜嗜沤沤冗冗伯伯颁颁帐帐从从焚焚六六辑辑匡匡国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述How do we Know the expectations of the FDA?FDAForm483FDAWarningLettersPersonalExperiences银银局局谜谜贡贡伤伤带带格格瞬瞬售售社社牧牧婴婴檬檬蟹蟹确确耸耸诛诛袍袍栅栅堆堆灶
50、灶餐餐疾疾伎伎怨怨横横霓霓家家部部偿偿威威魄魄国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述483 Observations There was inadequate method validation specificitydatatodemonstratethateachmethodwascapableofdistinguishingtheactiveingredientfromitsimpuritiesanddegradationproducts.Specificitystudiesdidnotincludethe
51、minimumstressconditions of acid and base hydrolysis, oxidation,thermal degradation and photolysis, degradationschematic for the active ingredient that identifies themajordegradationproductswasnotincludedforeachproduct.303020092009梧梧帜帜鸡鸡很很卢卢厌厌浩浩碳碳滴滴悸悸帧帧战战蘑蘑瀑瀑宅宅析析哼哼梯梯给给榜榜踪踪鼓鼓雄雄恨恨入入展展食食羚羚瓦瓦壹壹棉棉死死国国际际上上
52、不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述FDA Waning LetterOnadditiontotheexampleofmodifyingbothcompendialmethodsandcustomersuppliedmethods,wealsoobservedtheuseofunvalidatedin-housemethodsaswellasunvalidatedmodificationstoin-housemethods.Astatementindicatingthatthemethodhasnotbeenvalidat
53、edintheparticularformulationwasincludedinthecertificateofanalysisforuseofthisstatementdoesnotabsolvefromusingvalid,accurate,andreproduciblemethods.(June2000)313120092009绝绝磊磊帅帅吵吵绿绿玖玖现现敏敏析析篆篆沸沸恭恭更更哉哉插插纠纠蒸蒸棒棒篙篙籽籽体体洗洗血血直直饵饵淖淖试试叼叼寺寺裤裤兑兑靛靛国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述FDA Sys
54、tems Based Inspection:Laboratory System3232Method Method ValidationValidation13%13%Training/Qual.Training/Qual.4%4%Stability Program Stability Program 21%21%InadequateInadequateRecordsRecords27%27%Controls. GeneralControls. General35%35%Feb Feb July 2002: 212 Inspections (US) July 2002: 212 Inspecti
55、ons (US)* Reference: Albinus D* Reference: Albinus D Sa, FDA, CDER Office of Compliance, from AAPS, Nov. 2002 presentation. Sa, FDA, CDER Office of Compliance, from AAPS, Nov. 2002 presentation.20092009常常吏吏炮炮爽爽账账撂撂蹋蹋弓弓版版开开鸽鸽逝逝捅捅佛佛汉汉坎坎圈圈错错栓栓烧烧黄黄傻傻瘁瘁颠颠蹈蹈巳巳担担沤沤劲劲得得鲤鲤疫疫国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述Related Sitewww.fda.govwww.fda.gov/cder/卜卜肄肄郧郧柳柳搭搭徐徐端端害害庇庇獭獭弃弃弊弊彭彭锣锣展展凳凳劈劈刁刁盐盐武武虚虚季季镐镐吊吊唯唯俭俭答答超超泛泛穿穿臻臻嘴嘴国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述国国际际上上不不同同分分析析方方法法验验证证准准则则概概述述
