搜索
20106316、。3,4-(a)、。3,4-(a)[benzopyreneBap5,、、、、、、。。、、3,4-(a)。3,4-(a)5μg/kg,3,4-(a),,;、-,,。,3,4-(a),,。[1-3]-C18。11．1Supelco-Agilent1200JY92-RE-52A0.45μm3,4-(a)Sigma,99%、、、、、OrganomationC18Waters。,,,,313000:-3,4-,、C18。A=1424.54X-0.1367r=187.2%2.1%,0.4μg/kg,3,4-。3,4-(a)Determinationof3,4-benzoaPyreneinMeatproductsbyHighPerformanceLiquidChromatographyHUQi-jie,SHENLi-wei,QIMin,YAOTing,GONGYeHuzhouQualtySupervisionandInspectionStation,Huzhou313000Zhejiang,ChinaAbstract:Amethodwasdevelopedfordetermining3,4-benzoapyreneinmeatproducts,itncludedsonicationextraction,purificationbyliquid-liquiddistribution,anddecontaminationbyC18SPEcolumn,separationbyhighperformanceliquidchromatographywithafluorescentdetector.ThelinearequationwasA=1424.54X-0.1367,itscorrelationcoefficientwas1,itspercentrecoverywas87.2%,itsdefinitionwas2.1%,anddetectabilitywas0.4μg/kg.Themethodhadgoodisolationandsuitablefordeterminationof3,4-benzoapyrenein.KeywordsHPLC3,4-benzo[a]pyrenemeatproducts1981—。146201063161.2ZORBAXSB-C184.6×150mm,10μm+=90+10365nm410nm1mL/min;35℃5μL。1.31.3.13,4-(a)10.0mg100mLA100μg/mL。A5.00mL500mLB1μg/mL。B10mL0.00、0.002、0.01、0.10、0.50、1.00μg/mL。1.3.210g50mL2min10minKD50mL70℃20mL10mLKD。330mL1min30mL。10mL5mL15mLC185mL、10mL,30mL2mL0.45μmHPLC。22.13、、3。33,4-3,4-(a)。10g10、50、200ng3,4-(a)3。1。191.7%[3]6h~8h10min87.58%62.49%。3。2.23,4-(a)50mL、、、3,4-(a)4,2。290.55%,,、、[4]3,4-(a)。2.3C18、、[5]330mL。3。45mL33,4-(a)15mL。C18。C1813,4-(a)Table1Recoveryofthedifferentmethod3,4-(a)/ng10.0050.00200.0010.0050.00200.0010.0050.00200.003,4-(a)/ng9.1846.03182.408.7844.36172.465.9832.64124.80/%91.8092.0691.2087.8088.7286.2359.7965.2862.4023,4-(a)Table2Recoveryofthedifferentreagenttoextracting3,4-(a)/ng10.0050.00200.0010.0050.00200.0010.0050.00200.0010.0050.00200.003,4-(a)/ng9.0845.09181.328.7542.59175.237.2234.56148.617.5438.64144.80/%90.8090.1890.6687.5085.1887.6272.2069.1274.3075.4077.2872.4014720106316,,,C18。2。2.4、、、65%43,4-(a)4。65%65%。。2.5、、、3,4-a5μg/kg5μg/kg0.00、0.002、0.01、0.10、0.50、1.00μg/mL3,4-(a)1。13,4-a0.00~1.00μg/mLA=1424.54X-0.1367r=1。30.4μg/kg,3,4-a。20.004μg/mL3,4-a。5RSD2.1%86.4%,3,4-a。3、,3,4-(a),:10min,,C18,87.2%2.1%,0.4μg/kg。,3,4-(a),。,,,、,3,4-(a)。33,4-(a)Table3RecoveryofthedifferentmethodtopurifyingC183,4-(a)/ng10.0050.00200.0010.0050.00200.0010.0050.00200.003,4-(a)/ng8.4242.33170.728.6442.65174.533.2415.5668.54/%84.2084.6685.3686.4085.3088.7632.4031.1234.2743,4-(a)Table4Recoveryofthedifferentsolutiontoshampooing65%3,4-(a)/ng10.0050.00200.0010.0050.00200.0010.0050.00200.0010.0050.00200.003,4-(a)/ng6.9235.03137.588.7243.56174.535.2824.56101.218.5444.64180.12/%69.2070.0668.7987.2087.1287.2652.8049.1250.6085.4089.2890.0614820106316[1].GB/T5009．27-2003．(a)[S].,2004:137-142[2],,,.3,4-(a)[J].2007,30(4):140-143[3],,,.3,4-(a)[J].2007,28(2):251[4],,,.[J].2008,20(1):86-88[5],.[J].,1994,14(2):12-142009-07-22[1]Pb。。[2]。[3]*1000352mg/mL1mg/mL1∶1800℃1200℃。ResearchfortheEliminationofMatrixinterferenceontheDeterminationofLeadinCalciumNutrientSupplementsbyGFAASZHANGHua-junZHANGRong*BeijingInstituteForDrugControlBeijing100035,ChinaAbstract:Theinterferingfactorsofdeterminationofleadincalciumnutrientsupplementswerestudiedbasedonsamplecharacteristicsandtheroleofmatrixmodifiermechanism,selecttheammoniumdihydrogenphosphateandmagnesiumnitrateasmatrixmodifiertouse.Theoptimizeconditionsareasfollows:2mg/mLsolutionofammoniumdihydrogenphosphateandmagnesiumnitratesolution1mg/mLaproportionof1∶1toadd,ashingtemperatureto800℃,atomizationtemperature1200℃,therealizationofacalcium-basednutrientsupplementsintheleadcontentoftheexactquantitative.Keywords:calciumnutrientsupplements;leadtesting;theeliminationofinterference1981—。*。!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!149