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1、GC-MSScreenforthePresenceofMelamine(AdaptedfromFDA/ORAForensicChemistryCenterSOPT015)RevisedApril10,2007PURPOSE:Thisprocedureprovidesageneralguideforthesamplepreparationandanalysisofwheatglutenandpetfoodmatricesformelamineusinggaschromatography/massspectrometry.?Thisprocedureisdesignedtoscreenth
2、eTMSderivativeofamethanolextractofthesampleanditincorporatesinstrumentalparameterswhichpermit10.5minuteruntimes.SCOPE:Thisprocedureisapplicabletodrywheatgluten,drypetfood,andwet“cutsandgravy”typepetfood.?Thisprocedureinvolvesextractionsinmethanolandthereforepreselectscompoundswhicharesolubleorpa
3、rtiallysolubleinmethanol.?Duetosolubilitylimitationsofmelamineinmethanol,thismethodisintendedtobeaqualitativescreenonly.RESPONSIBILITY:Itistheresponsibilityoftheanalysttonoteanymodificationstothisprocedureintheworksheet.DEFINITIONSANDACRONYMS:TMS–trimethylsilylSAFETYCONSIDERATIONS:Acceptedsafety
4、measuresshouldbeemployedwhenworkingwithchemicalsandpressurizedgases.EQUIPMENT:Agilent5975GC-MSsystemequippedwitha30mDB-5MScolumn(orequivalent)Reacti-Vap–Evaporating/HeatingModuleREAGENTS:Methanol:HPLCgradePyridine:CertifiedA.C.S.BSTFAwith1%TMCS:bis(trimethylsilyl)trifluoroacetamidewith1%Trimethy
5、lchlorosilane(e.g.SylonBFT,Supelco)QCELEMENTS:Ablankshouldberunattheonsetofeachanalysisandthenrandomlythroughouttheanalysisifthereissuspicionofcarryover.?Afortifiedsample(seePartC)shouldbeanalyzedwitheachsetofsamplestodemonstrateeffectivesystemperformance.PROCEDURES(PROCESSDETAILS):Thisprocedure
6、maybeusedwiththeGCoperatingineitherthesplitlessorsplit(1:20)mode.?Generally,thesplitlessmodeisadvisableforsampleswheremoresensitivityisrequired.??Thesplitmodeissuitablewheresampleavailabilityisnotlimitedandtherecommendedamountcanbeprepared(~0.5gsamplepreparations).A.MethanolExtract(Underivatized
7、Extract):UnknownWheatGluten/PetFoodSamples:?Transferapproximately0.500gofthesampleintoa20mlscintillationvialandadd5mlmethanol.?Vortexbrieflytomix,thensonicatefor10minutes.?Centrifugeforapproximately6minutesat4500rpmandthenfi
