Chapter 1 Regulatory Operations

SECTION100PesticideAnalyticalManualVol.I100–1TransmittalNo.98-1(10/97)FormFDA2905a(6/92)TableofContentspagedate101:RegulatoryPolicy101A:RegulatoryAuthority101-11/94101B:RegulatoryOperations101-21/94101C:Monitoring101-31/94References101-31/94102:PreparationofAnalyticalSamples102A:Introduction102-11/94102B:PortionofFoodCommodityto102-11/94beAnalyzedRawAgriculturalCommodities102-11/94ProcessedFoods102-41/94102C:CompositingandComminutingthe102-51/94LaboratorySampleChapter1RegulatoryOperationsChapter2GeneralAnalyticalOperationsandInformationChapter3MulticlassMRMsChapter5GLCChapter4SelectiveMRMsChapter6HPLCSECTION100TransmittalNo.98-1(10/97)FormFDA2905a(6/92)100–2PesticideAnalyticalManualVol.Ipagedate102D:HandlingSamplesforSpecialAnalyses102-61/94102E:RetentionofReservePortions102-61/94References102-61/94103:MethodApplicationinRegulatoryAnalysis103A:Introduction103-11/94103B:ChoiceofMethod103-11/94PAM103-11/94Other“Official”Methods103-21/94OtherPublishedMethods103-21/94103C:TentativeIdentification103-31/94103D:ResidueQuantitation103-31/94103E:ConfirmationofIdentity103-41/94103F:Documentation103-61/94AnalyticalReports103-61/94Chromatograms103-71/94ChromatographicData103-71/94References103-81/94104:AnalyticalResults104A:Introduction104-11/94104B:Reporting104-11/94PortionofCommodity104-11/94NatureoftheResidue104-21/94ResiduesMeasuredfromDerivative104-21/94orBreakdownProductSignificantFigures104-31/94Trace104-31/94Confirmation104-41/94104C:DeterminingCompliancewithRegulations104-41/94GeneralRuleforMulticomponentResidues104-41/94SpecialSituations104-41/94References104-51/94105:AnalyticalLimitsofQuantitation105A:Definition105-110/97105B:Calculation105-110/97105C:Implementation105-210/97105D:FactorsAffectingTargetLimitsofQuantitation105-210/97SECTION100PesticideAnalyticalManualVol.I100–3TransmittalNo.98-1(10/97)FormFDA2905a(6/92)pagedateFigures102-a:FractionofCheeseUnitstoTakefor102-51/94CompositingTables102-a:PortionofRawAgriculturalCommodity102-21/94tobeAnalyzedforPesticideResidues102-b:PortionofProcessedFoodtobeAnalyzed102-49/96forPesticideResidues103-a:InformationProvidedbyUseofElement-103-51/94SelectiveDetectors104-a:PortionofCommodityforCalculation104-21/94andReportingofResidueLevels105-a:ExamplesofMethodSpecifications105-410/97UsedtoCalculateLqsSECTION100TransmittalNo.98-1(10/97)FormFDA2905a(6/92)100–4PesticideAnalyticalManualVol.IPesticideAnalyticalManualVol.ISECTION101TransmittalNo.94-1(1/94)FormFDA2905a(6/92)101–1101:REGULATORYPOLICYTheexpressedpurposeofthePesticideAnalyticalManualistopublishanalyticalmethodologyusedbytheFDAinenforcingpesticidetolerances.TounderstandFDA’sapplicationofmethodologypublishedinthemanual,itisimportanttounderstandpesticidetoleranceregulationsandrelatedFDAregulatoryoperations.MaterialinChapter1reflectsFDAregulatorypoliciesthataffectitsapplicationofanalyticalmethodology.101A:REGULATORYAUTHORITYInformationrelatedtoandthecharacteristicsofpesticidetolerancesincludethefollowing:Atoleranceisthemaximumconcentrationofapesticideresiduethatislegallypermittedtoremaininafood.Thetoleranceisnotexpectedtobeexceededifthepesticide’sregisteredusedirectionsarefollowed.ThestatutoryauthorityfortheEnvironmentalProtectionAgency’s(EPA’s)establishmentoftolerancesisprovidedbysections408and409oftheFederalFood,Drug,andCosmeticAct.TolerancesestablishedbyEPAaresetforthinTitle40oftheCodeofFederalRegulations(CFR),Part180forrawagriculturalcommodities,Part185forprocessedfood,andPart186foranimalfeed.Theconcentrationoftoler-anceslistedin40CFR180,185,and186isexpressedintermsofppm(i.e.,mgpesticideresidue/kgfood).Inaddition,certainpesticidesareexemptedfromtheneedfortolerances;suchexemptionsarelistedin40CFR180.1001.Atoleranceforapesticideresidueonarawagriculturalcommodity,e.g.,tomatoes,alsoappliestoprocessedformsofthatcommodity,e.g.,cannedtomatoes.Incaseswhereprocessingmayconcentratetheresidue,afoodadditiveregulationmaybeissuedin40CFRPart185toestablishahighertoleranceonthatprocessedcommodity,e.g.,tomatopaste.Atoleranceregulationspecifiesthecompositionofpesticideresidueforwhichthelimitapplies;i.e.,atolerancecanapplytotheparentformoftheactiveingredientonly,parentcompoundplusoneormoremetabolitesand/ordegradationproducts,oneormoremetabolitesand/ordegrada-tionproductsonly,orsomechemicalmoietythatcanbemeasuredanalyti-callyforcalculatingthepesticideresidue.Achemicalentitynotspecifiedbythetoleranceregulationisnotincludedintheresiduefortoleranceenforcementpurposes(Section104).Atoleranceregulationalsospecifieseachindividualfood(e.g.,apples)orfoodgroup(e.g.,citrusfruit)towhichthelimitapplies.Notoleranceexistsforaresidueonacommodityunlessthecommodityitselforthegrouptowhichitbelongsisspecified.Intheexaminationofafoodlottodeterminewhetheritcomplieswithtolerances,itisnecessarytoprovideasampleforanalysisthatisrepresen-tativeofthelotinordertodeterminetheaveragepesticideresiduecontentPesticideAnalyticalManualVol.ISECTION101101–2TransmittalNo.94-1(1/94)FormFDA2905a(6/92)ofthelot.Tolerancesapplytothatsampleorarepresentativeportionofthatsample.