蔬菜中多溴联苯醚的定量测定及其对人体的生物有效性

28120091FENXICESHIXUEBAO(JournalofInstrumentalAnalysis)Vol128No1116:2008-07-26;:2008-10-13:(2008CB418205);(OGL-200704):(1984-),,,:,Tel:[phone],E-mail:yuyingxin@staff1shu1edu1cn1,1,1,1,2,1,3,1,3(1.,200444;2.,200444;3.,510640):,-,13(PBDEs)GC-NCIMS,5141517pg/g,RSD78%97%016%1010%PBDEs,PBDEs42411pg/g98113pg/g,3315%216%,13PBDEs13216pg/g2611pg/g,:;;;:X132;O657163:A:1004-4957(2009)01-0001-06DeterminationofPolybrominatedDiphenylEthersinVegetableandTheirBioaccessibilitytoHumanLUMin1,HANShu2yuan1,YUYing2xin1,ZHANGDong2ping1,WUMing2hong2,SHENGGuo2ying1,3,FUJia2mo1,3(1.InstituteofEnvironmentalPollutionandHealth,SchoolofEnvironmentalandChemicalEngineering,ShanghaiUniversity,Shanghai200444,China;2.InstituteofAppliedRadiation,SchoolofEnvironmentalandChemicalEngineering,ShanghaiUniversity,Shanghai200444,China;3.StateKeyLaboratoryofOrganicGeochemistry,GuangzhouInstituteofGeochemistry,ChineseAcademyofSciences,Guangzhou510640,China)Abstract:Amethodfor13polybrominateddiphenylether(PBDEs)detectioninvegetablewasdevel2oped.ThesamplesweretreatedbySoxhletextraction,andcleanedupbygelpermeationchromatog2raphycolumnandmultilayersilica-aluminacolumn.Thedetectionofanalyteswasperformedbygaschromatographymassspectrometrynegativeionchemicalionizationdetection(GC-NCIMS).Theresultsshowedthatthedetectionlimitsof13tri2tohepta2BDEswereintherangeof514-1517pg/gdryweight.Therecoverieswerebetween78%and97%withRSDof016%-1010%.Inaddition,thebioaccessibilityofPBDEsinthesimulatinghumangastrointestinaltractwereinvestigated.TheconcentrationsofPBDEsincarrotandspinachwere42411pg/gand98113pg/g,andtheaveragebioaccessibilitywere3315%and216%,respectively.ThetotalbioaccessibleconcentrationsofPB2DEsincarrotandspinachwere13216pg/gand2611pg/g,respectively.Theobtainedresultsmayprovideusefulinformationforpollutantexposureassessmenttohuman.Keywords:polybrominateddiphenylether(PBDEs);vegetable;invitrotest;bioaccessibility,(polybrominateddiphenylether,PBDEs)[1-2]28PBDEs,[3-6]PBDEs[7-8],,,PBDEs,[9-10]PBDEs[11-12],(bioavailability),(invitrotest),,,37,,(bioaccessibility),[13-14][15-18]PBDEs,[19]PBDEs,(QA/QC),PBDEs,,PBDEs,1111PBDEs(BDE17287147661009985154153138183190209)AccuStandard13C2PCB14113C2PCB208(CambridgeIsotopeLaboratories)(+)2Fluka;D2(+)2(Sig2maUltra,9915%,)Sigma;Merck,(01150125mm)(010750115mm)72h,,18025012h3%()25%()NaOH(1mol/L)44%()H2SO4,01037401075mmS2X3(Bio-BeadsS2X3)Rio-RadMilliporeElix,12125min112PBDEs,,0118mm5g,13C2PCB141(4L1mg/L),250mL-(11)72h1mL,[19](GPC,01037401075mmS2X3),GPC-(11),115mL,115280mL,200mL1mL,-[20]:6cm2cm5cm2cm6cm2cm70mL-(11),13C2PCB2082mL,100L,411311311[21-22]:1L1g(arabinogalactanfromlarchwood)2g(pectinfromapples)1g(xylanfrombirchwood)3g(potatostarch)014gD2(+)23g(yeastextract)1g(peptonefrompoultry)4g(mucinfromporcinestomach,type)015gL2(L2cysteine),12115min:1L011molL-1HCl,0109g700FIP-Ug-1(pepsinfromporcinegastricmucosa),800mL100mLpH310011:1L1215gNaHCO3610g(bilebovine)019g(pancreatinfromporcinepancreas,350FIP-Ug-1(activated)protease,6000FIP-Ug-1lipase,7500FIP-U21:g-1amylase),11312,[22]114(NCI)6890N-5975-(GC/MS,Agilent),,280,1L,(SIM);DB25MS(30m0125m0125m,J&WScientific,USA),110mLmin-1,:1101min8min-1180,1min,2min-1240,5min,2min-1280,5min,20min-1300,15min,30010minm/z7981,13C2PCB141m/z372374;13C2PCB208m/z476478PBDEs11PBDEsFig11GC-NCIMS/SIMchromatogramsofPBDEsinstandard,blanksample,carrotsampleandspinachsample115,7(2100g/L),,,0199922115,6s,3136s(IDL)BDE17287147661009985154153138183190013015015013015016013018013014016014019pg,5g,100L,(MDL)6181019101461310171211514151761981812117191117pg/g328212,PBDEs1,PBDEs78%92%,016%718%;13C2PCB141(87119)%BDE47BDE99,13PBDEs80%97%,13C2PCB14190%,10%BDE209,,1PBDEsTable1TherecoveriesofPBDEsinspikedblankandcarrotsampleCompoundRecoveryR/%(AverageRSD)BlanksampleCarrotsampleCompoundRecoveryR/%(AverageRSD)BlanksampleCarrotsampleBDE177821080716BDE859021389219BDE288011682713BDE1548431387314BDE718401687411BDE1538901988217BDE4779710841010BDE1389231690316BDE668611697919BDE1838471886915BDE1008401788411BDE1908641087218BDE99866118931413C2PCB1418711990113213PBDEs2,13C2PCB14111413%8818%,115%,BDE172871476610099154153138183,BDE47,BDE71BDE99,BDE85BDE190,BDE85,,,;[23],,[24-25],PBDEs,BDE47BDE99[26]PBDEs42411pg/g98113pg/g,,,,,PBDEs,Ohta[27]2PBDEsTable2TheconcentrationsofPBDEsincarrotandspinachsamplepg/gCompoundCarrotSpinachAverageSDRSDsr/%AverageSDRSDsr/%BDE179170177101610114818BDE284180112182811116518BDE7179112102151141917121510BDE47257162191114681160141219BDE665190181318818019917BDE1009170176182811211715BDE992215116619141181215818BDE85ND3NDBDE15441801511113111113411BDE153141511061978108121015BDE13851201510101815018411BDE18310151151410321400101BDE190ND1516114911PBDEs424112180179811347144183belowthedetectionlimit()214[17],(PBDEs41:PBDEs),PBDEs(3)PBDEs2311%3910%,3315%,211%219%,216%Kulkarni[28],,100g2014g,1115g[29],PBDEs2Xing[17],PCBs25%,,Oomen[30]5,pH,,3PBDEsTable3ThebioaccessibilitiesofPBDEsincarrotandspinachtohumanandtheirbioaccessibleconcentrationsCompoundCarrotBioaccessibilities(Average/%SD)3Bioaccessibleconcentrationw/(pgg-1)33Spinach