CACGL 90-2017 食品和饲料中农药残留测定分析方法的性能标准指南

GUIDELINESONPERFORMANCECRITERIAFORMETHODSOFANALYSISFORTHEDETERMINATIONOFPESTICIDERESIDUESINFOODANDFEEDCAC/GL90-2017Adoptedin2017.CAC/GL90-20172OBJECTIVE1.Thepurposeoftheseguidelinesistodefineanddescribetheperformancecriteria,whichshouldbemetbymethodstoanalysepesticideresiduesinfoodsandfeed(hereafterreferredtoasfood).Itaddressesthecharacteristics/parameterstoprovidescientificallyacceptableconfidenceintheanalyticalmethodthatisfitfortheintendeduseandmaybeusedtoreliablyevaluatepesticideresiduesforeitherdomesticmonitoringand/orinternationaltrade.2.Thisdocumentisapplicabletobothsingleresiduemethodsandmulti-residuemethods(MRMs)thatanalysetargetcompoundsinallfoodcommoditiespertheresiduedefinition.3.Theseguidelinescoverqualitativeandquantitativeanalyses,eachhavingtheirownmethodperformancecriteria.Performancecriteriaofmethodsforanalyteidentificationandconfirmationarealsoaddressed.PRINCIPLESFORTHESELECTIONANDVALIDATIONOFMETHODSA.DefiningthePurposeoftheMethodandScope4.Theintendedpurposeofthemethodisusuallydescribedinastatementofscope,whichdefinestheanalytes(residues),thematrices,andtheconcentrationranges.Italsostateswhetherthemethodisintendedforscreening,quantification,identification,and/orconfirmationofresults.5.Inregulatoryapplications,themaximumresiduelimit(MRL)isexpressedintermsoftheresiduedefinition.Residueanalyticalmethodsshouldbeabletomeasureallcomponentsoftheresiduedefinition.6.Fitness-for-purposeistheextenttowhichtheperformanceofamethodmeetstheend-user’sneeds,andmatchesthecriteria(dataqualityobjectives)agreedbetweenthelaboratoryandtheend-user(orclient)ofthedata,withintechnicalandresourceconstraints.Fitness-for-purposecriteriacouldbebasedonsomeofthecharacteristicsdescribedinthisdocument,butultimatelywillbeexpressedintermsofacceptablecombineduncertainty1.7.Selectionofmethodsisbasedonanalytesandtheintendedpurposeoftheanalyses2.B.SupplementingotherCodexAlimentariusCommissionGuidelines8.TheCodexAlimentariusCommission(CAC)hasissuedaguideline3forlaboratoriesinvolvedinthetestingoffoodsforimport/exportwhichrecommendsthatsuchlaboratoriesshould:(a)useinternalqualitycontrolprocedures,suchasthosedescribedinthe“HarmonizedGuidelinesforInternalQualityControlinAnalyticalChemistryLaboratories;”(b)participateinappropriateproficiencytestingschemesforfoodanalysiswhichconformtotherequirementlaidoutin“TheInternationalHarmonizedProtocolforProficiencyTestingof(Chemical)AnalyticalLaboratories(PureAppl.Chem.,vol78,No.1,pp.145-186,2006);”and(c)wheneveravailable,usemethodswhichhavebeenvalidatedaccordingtoprinciplesprovidedbytheCAC.9.Theanalyticalmethodsshouldbeusedwithintheinternationallyaccepted,approved,andrecognizedlaboratoryQualityManagementSystem4tobeconsistentwiththeprinciplesinthedocumentforqualityassurance(QA)andqualitycontrol(QC)referencedabove.C.MethodValidation10.Theprocessofmethodvalidationisintendedtodemonstratethatamethodisfit-for-purpose.Thismeansthatwhenatestisperformedbyaproperlytrainedanalystusingthespecifiedequipmentandmaterialsandexactlyfollowingthemethodprotocol,accurate,reliable,andconsistentresultscanbeobtainedwithinspecifiedstatisticallimitsforsampleanalysis.Thevalidationshoulddemonstratetheidentityandconcentrationoftheanalyte,takingintoaccountformatrixeffects,provideastatisticalcharacterizationofrecoveryresults,andindicateifthefrequencyoffalsepositivesandnegativesareacceptable.Whenthemethodisfollowedusingsuitableanalyticalstandards,resultswithintheestablishedperformancecriteriashouldbeobtainedonthesameorequivalentsamplematerialbyatrainedanalystinanyexperiencedresiduetestinglaboratory.Toensuremethodperformanceremainsappropriateovertime,methodvalidationshouldbecontinuouslyassessed(e.g.recoveryspikes).1HarmonizedIUPACGuidelinesForSingle-LaboratoryValidationofMethodsofAnalysis,Pure&Appl.Chem.,74(5),2002;835–8552OECDGuidanceDocumentonPesticideResidueAnalyticalMethods,ENV/JM/MONO(2007)173GuidelinesfortheAssessmentoftheCompetenceofTestingLaboratoriesInvolvedintheImportandExportControlofFood(CAC/GL27-1997)4Generalrequirementsforthecompetenceoftestingandcalibrationlaboratories,ISO/IEC17025(2005).CAC/GL90-20173PERFORMANCEPARAMETERSFORANALYTICALMETHODS11.Thegeneralrequirementsfortheindividualperformancecriteriaofamethodaresummarizedbelow1,5A.MethodDocumentation12.Aftervalidation,themethoddocumentationshouldprovide,inadditiontoperformancecriteria(dataqualityobjectives),thefollowinginformation:(a)Identityoftheanalytesincludedintheresiduedefinition.(b)Concentrationrangecoveredbythevalidation;(c)Matricesusedinthevalidation(representativecommoditycategories,e.g.,similaragriculturalproductsbasedoncharacteristicsincludingmoisture,fat,andsugarcontent,pH);(d)Protocoldescribingtheequipment,reagents,detailedstep-by-stepprocedureincludingpermissiblevariations(e.g.“heatat100±5°Cfor30±5min”),calibrationandqualityprocedures,specialsafetyprecautionsrequired,andintendedapplicationandcriticaluncertaintyrequirements;(e)quantitativeresultoftheexpandedmeasurementuncertainty(MU)forthemethodshouldbecalculatedinthevalidationprocedureandreported,ifr