FDA-Method of Test for Phthalate Plasticizers in Foods

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1、MethodofTestforPhthalatePlasticizersinFoods(Draft)1.ScopeThismethodisapplicableforthedeterminationofphthalatesinfoods.2.MethodAfterextraction,phthalatesaredeterminedbyliquidchromatograph/tandemmassspectrometer(LC/MS/MS).2.1.Equipment2.1.1.Liquidchromatograph/tandemmassspectrom

2、eter.+2.1.1.1.Ionsource:positiveionelectrosprayionization,ESI.2.1.1.2.Column:ACQUITYBEHC18,1.7μm,2.1mmi.d.×100mm,orequivalentproduct.2.1.2.Sonicator.2.1.3.Centrifuge:rotationspeed≧3500ppm.2.1.4.Vortexmixer.2.2.ChemicalsMethanol,HPLCgrade;Ammoniumacetate,ARgrade;Mili-Qwater,res

3、istivity≧18MΩ‧cm(@25℃);Benzylbutylphthalate(BBP),referencestandard;Dibutylphthalate(DBP),referencestandard;Di(2-ethylhexyl)phthalate(DEHP),referencestandard;Di-n-octylphthalate(DNOP),referencestandard;Diisononylphthalate(DINP),referencestandard;Diisodecylphthalate(DIDP),refere

4、ncestandard.2.3.Apparatus2.3.1.Glassburette:1mLand5mL.2.3.2.Glassvolumetricflask:10mLand50mL.2.3.3.Glasscentrifugetube:10mL.Note:allapparatususedfortestingshouldbemadebyglassnotplastics,andneedberinsedbymethanolanddriedbeforeuse.2.4.Reagents2.4.1.5mMAmmoniumacetatesolutionDiss

5、olve0.39gofammoniumacetateinMili-Qwateranddiluteto1000mL.2.4.2.Mobilephasesolution1Methanol:5mMammoniumacetatesolution(9:1,v/v).2.5.StandardsolutionpreparationAccuratelyweigh50mgofBBP,DBP,DEHP,DNOP,DINPandDIDPreferencestandardtoeach50-mLvolumetricflask,dissolveanddilutetovolum

6、ewithmethanolasstandardstocksolution.Transfer0.25mLofeachstandardstocksolutionintoa50-mLvolumetricflaskanddilutetovolumewithmethanolasmixedstocksolution.Whentouse,dilutemixedstocksolutionwithmethanolto0.02~0.5μg/mLasworkingstandardsolution.2.6.SamplesolutionpreparationTransfer

7、about1gofthesampleaccuratelyweighedtoa50-mLvolumetricflaskandadd45mLofmethanol,sonicatefor30min.,thencooltoroomtemperature,dilutewithmethanoltovolumeandmix,standstillforseveralminutes,transferabout5mLoftheuppersolutiontoacentrifugetube,andcentrifugeat3500rpmfor10min.Usethesupe

8、rnatantasthesamplesolution.2.7.Identificationandquantificatio