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1、GC-MSScreenforthePresenceofMelamineandCyanuricAcid(formerlytitledGC-MSScreenforthePresenceofMelamine)(AdaptedfromFDA/ORAForensicChemistryCenterSOPT015)TitleRevisedApril25,2007PURPOSE:Thisprocedureprovidesageneralguideforthesamplepreparationandanalysisofwheatglutenandpetfoodmatricesformelamine
2、usinggaschromatography/massspectrometry.?ThisprocedureisdesignedtoscreentheTMSderivativeofamethanolextractofthesampleanditincorporatesinstrumentalparameterswhichpermit10.5minuteruntimes.SCOPE:Thisprocedureisapplicabletodrywheatgluten,drypetfood,andwet“cutsandgravy”typepetfood.?Thisprocedurein
3、volvesextractionsinmethanolandthereforepreselectscompoundswhicharesolubleorpartiallysolubleinmethanol.?Duetosolubilitylimitationsofmelamineinmethanol,thismethodisintendedtobeaqualitativescreenonly.RESPONSIBILITY:Itistheresponsibilityoftheanalysttonoteanymodificationstothisprocedureintheworksh
4、eet.DEFINITIONSANDACRONYMS:TMS–trimethylsilylSAFETYCONSIDERATIONS:Acceptedsafetymeasuresshouldbeemployedwhenworkingwithchemicalsandpressurizedgases.EQUIPMENT:Agilent5975GC-MSsystemequippedwitha30mDB-5MScolumn(orequivalent)Reacti-Vap–Evaporating/HeatingModuleREAGENTS:Methanol:HPLCgradePyridine
5、:CertifiedA.C.S.BSTFAwith1%TMCS:bis(trimethylsilyl)trifluoroacetamidewith1%Trimethylchlorosilane(e.g.SylonBFT,Supelco)QCELEMENTS:Ablankshouldberunattheonsetofeachanalysisandthenrandomlythroughouttheanalysisifthereissuspicionofcarryover.?Afortifiedsample(seePartC)shouldbeanalyzedwitheachsetofs
6、amplestodemonstrateeffectivesystemperformance.PROCEDURES(PROCESSDETAILS):ThisproceduremaybeusedwiththeGCoperatingineitherthesplitlessorsplit(1:20)mode.?Generally,thesplitlessmodeisadvisableforsampleswheremoresensitivityisrequired.??Thesplitmodeissuitablewheresampleavailabilityisnotlimitedandt
7、herecommendedamountcanbeprepared(~0.5gsamplepreparations).A.MethanolExtract(UnderivatizedExtract):UnknownWheatGluten/PetFoodSamples:?Transferapproximately0.500gofthesampleintoa20mlscintillationvialandadd5mlmethanol.?Vortexbrieflytomix,thenson
