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1、FDA/ORA/DFSLaboratoryInformationBulletinNo.4475Page1of39SCREENFORTHEPRESENCEOFPOLYCYCLICAROMATICHYDROCARBONSINSELECTSEAFOODSUSINGLC-FLUORESCENCE1*1111SamuelGratz,AngelaMohrhaus,BryanGamble,JillGracie,DavidJackson,John11111Roetting,LauraCiolino,HeatherMcCauley,GerrySchneider,DavidCrockett,22233Wal
2、terKrol,TerriArsenault,JasonWhite,MicheleFlottmeyer,YokoJohnson,11DouglasHeitkemper,FredFricke1ForensicChemistryCenter(FCC),FoodandDrugAdministration,6751StegerDrive,Cincinnati,OH452372DepartmentofAnalyticalChemistry,ConnecticutAgriculturalExperimentStation3LaboratoryServicesDivision,MinnesotaDep
3、artmentofAgricultureAbstractAliquidchromatography-fluorescencedetection(LC-FLD)methodhasbeendevelopedtoscreenforfifteentargetedparentpolycyclicaromatichydrocarbons(PAHs)atconcentrationsbelowtheestablishedFDAlevelsofconcerninoysters,shrimp,crabs,andfinfish.Theprocedurewasvalidatedbyspikerecoveryex
4、perimentsofthefifteenparentPAHsatthreelevelsforeachmatrix,withrecoveriesrangingfrom78–99%.Additionalspikerecoveryexperimentswereconductedforaseriesofalkylatedhomologsofnaphthalene,dibenzothiophene,andphenanthrene,withrecoveriesrangingfrom87–128%.MethodaccuracywasalsoevaluatedbasedonanalysisofNati
5、onalInstituteofStandardsandTechnology(NIST)StandardReferenceMaterial(SRM)1974b.PAHsareextractedusingamodificationofthequick,easy,cheap,effective,rugged,andsafe(QuEChERS)samplepreparationprocedure,employingacetonitrile(CH3CN)asthesolvent.Theextractsarefilteredusing0.2micronsyringefilters,butrequir
6、enopost-extractionsamplecleanupforLC-FLDanalysis.ThechromatographicmethodemploysapolymericC18stationaryphasedesignedforPAHanalysiswithgradientelutiontoresolvefifteentargetedPAHsina35minuteruntime.Fortheanalysisofunknowns,asamplethatisdeterminedtobepositiveforatargetedPAHatorabove50%oftheFDAlevelo
7、fconcernrequiresthatfurthertestingand/orconfirmationbeperformed.Additionally,anestimateoftotalPAHconcentrationincludingalkylatedhomologsinthesampleiscalculated.SamplescontainingtotalPAHconcentrationsgreaterthan50%ofthe
