Chapter 3 Multiclass MRMs

SECTION100PesticideAnalyticalManualVol.I300–1TransmittalNo.2000-1(10/1999)FormFDA2905a(6/92)TableofContentspagedate301:MulticlassMRMs:ConceptandApplication301A:RecommendedApplicationofMulticlassMRMs301-11/94301B:CapabilitiesandLimitationsofMRMs301-41/94InfluenceofSolventsonMethodology301-41/94Extraction301-41/94Cleanup301-61/94DeterminativeSteps301-71/94References301-71/94302:MethodIforNonfattyFoodsBasicReferences302-11/94GeneralPrinciples302-11/94Applicability302-11/94MethodModules302-11/94Validation302-51/94Chapter1RegulatoryOperationsChapter2GeneralAnalyticalOperationsandInformationChapter3MulticlassMRMsChapter5GLCChapter4SelectiveMRMsChapter6HPLCTransmittalNo.2000-1(10/1999)FormFDA2905a(6/92)300–2SECTION100PesticideAnalyticalManualVol.IE1Extractionwithacetone,liquid-liquidpartitioningwithpetroleumether/methylenechloride302-71/94E2Extractionwithacetone,removalofwaterwith40gHydromatrix302-91/94E3Extractionwithacetone,removalofwaterwith25gHydromatrix302-121/94E4Extractionwithwater/acetone,liquid-liquidpartitioningwithpetroleumether/methylenechloride302-131/94E5Extractionwithacetone,liquid-liquidpartitioningwithacetone/methylenechloride302-1510/99E6Extractionwithwater/acetone,liquid-liquidpartitioningwithacetone/methylenechloride302-1510/99E7Extractionwithacetoneandsolidphaseextractioncartridges,liquid-liquidpartitioning302-1710/99C1Florisilcolumn(4g)cleanup,withonemethylenechlorideeluant302-191/94C2Charcoal/Celite/magnesiumoxidecolumncleanup302-211/94C3Charcoal/SilanizedCelitecolumncleanup302-231/94C4C-18cartridgecleanup302-251/94C5Florisilcolumncleanup,withmixedethereluants302-271/94C6SAX/PSAcartridgecleanup302-2910/99Determination302-3110/97Confirmation302-321/94DG1GLC,100%methylsiloxane,200C,EC302-331/94DG2GLC,100%methylsiloxane,200C,FPD-P302-3510/97DG3GLC,100%methylsiloxane,200C,ELCD-X302-371/94DG4GLC,100%methylsiloxane,200C,ELCD-N302-391/94DG5GLC,100%methylsiloxane,200␣C,N/P302-4110/97DG6GLC,100%methylsiloxane,130C,FID302-431/94DG7GLC,100%methylsiloxane,130C,EC302-451/94DG8GLC,100%methylsiloxane,130C,FPD-P302-471/94DG9GLC,100%methylsiloxane,130C,ELCD-X302-491/94DG10GLC,100%methylsiloxane,230C,EC302-511/94DG11GLC,100%methylsiloxane,230C,FPD-P302-531/94DG12GLC,100%methylsiloxane,230C,ELCD-X302-551/94DG13GLC,50%phenyl,50%methylsiloxane,200C,EC302-571/94pagedateSECTION100PesticideAnalyticalManualVol.I300–3TransmittalNo.2000-1(10/1999)FormFDA2905a(6/92)DG14GLC,50%phenyl,50%methylsiloxane,200C,FPD-P302-5910/97DG15GLC,50%phenyl,50%methylsiloxane,230C,FPD-S302-611/94DG16GLC,50%phenyl,50%methylsiloxane,200C,ELCD-X302-631/94DG17GLC,50%phenyl,50%methylsiloxane,200C,N/P302-6510/97DG18GLC,50%cyanopropylphenyl,50%methylsiloxane,200C,EC302-671/94DG19GLC,50%cyanopropylphenyl,50%methylsiloxane,200C,FPD-P302-691/94303:MethodIIforNonfattyFoodsBasicReferences303-11/94GeneralPrinciples303-11/94Applicability303-11/94MethodModules303-11/94Validation303-31/94E1Extractionwithacetonitrile,partitionintopetroleumether303-71/94E2Extractionfromeggswithacetonitrile,partitionintopetroleumether303-81/94E3Extractionwith35%water/acetonitrile,partitionintopetroleumether303-91/94E4Extractionwithacetonitrileandwater,partitionintopetroleumether303-91/94E5Extractionwithheatedacetonitrileandwater,partitionintopetroleumether303-101/94C1Florisilcolumncleanup,withthreeethylether/petroleumethereluants303-111/94C2Florisilcolumncleanup,withthreemethylenechlorideeluants303-121/94Determination303-131/94Confirmation303-131/94304:MethodforFattyFoodsBasicReference304-11/94GeneralPrinciples304-11/94Applicability304-11/94MethodModules304-11/94Validation304-31/94E1Extractionoffatwithsodiumsulfate,petroleumether304-51/94E2Smallscaleextractionoffatwithsodiumsulfate,petroleumether304-71/94pagedateTransmittalNo.2000-1(10/1999)FormFDA2905a(6/92)300–4SECTION100PesticideAnalyticalManualVol.IE3Extractionoffatbyfiltering304-91/94E4Extractionoffatwithsolventsfromdenaturedproduct304-111/94E5Extractionoffatwithsolvents304-131/94C1Acetonitrile-petroleumetherpartitioning,Florisilcolumncleanup,threemixedethereluants304-151/94C2Acetonitrile-petroleumetherpartitioning,Florisilcolumncleanup,threemethylenechlorideeluants304-181/94C3Acetonitrile-petroleumetherpartitioning,Florisilcolumncleanup,petroleumetherandthreemixedethereluants304-191/94C4Acetonitrile-petroleumetherpartitioning,Florisilcolumncleanup,petroleumetherandthreemethylenechlorideeluants304-191/94C5Gelpermeationchromatography(GPC)304-211/94C6GPC,Florisilcolumn(4g)cleanup,threemethylenechlorideeluants304-241/94C7Florisilcolumn(4g)cleanup,twomixedethereluants,optionalalkalinehydrolysis304-271/94C8Dispersiononalumina,Florisilcolumncleanup,threemixedethereluants304-291/94C9Dispersiononalumina,Florisilcolumncleanup,threemethylenechlorideeluants304-321/94Determination304-331/94Confirmation304-331/94Figures301-aRecommendedApproachtoAnalysisofFoods301-21/94302RecommendedApproach:NonfattyFoods302-410/99303-aRecommendedApproach:NonfattyFoods303-31/94304-aRecommendedApproach:FattyFoods304-31/94304-bDeliv