固相萃取_固相微萃取_气相色谱法测定饮用水中多溴联苯醚

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1、2362012,Vol.33,No.08食品科学※分析检测固相萃取/固相微萃取-气相色谱法测定饮用水中多溴联苯醚何迎春1，王正虹2，李林1,*，周倩如2(1.西南大学食品科学学院，重庆400716；2.重庆市疾病预防控制中心，重庆400042)摘要：目的：建立固相萃取/固相微萃取-气相色谱法测定饮用水中多溴联苯醚(BDE-47和BDE-99)含量的新方法。方法：固相萃取-气相色谱直接取水样100mL，过LC-C18柱，经正己烷洗脱，洗脱液于80℃水浴挥干，异辛烷定容至1mL，直接进样1μL测定，该法对B

2、DE-47和BDE-99的检出限分别为0.0008μg/L和0.0009μg/L，回归方程相关系数分别为0.9996和0.9997，RSD(n＝6)分别为1.0%～4.9%和0.96%～4.4%；固相微萃取-气相色谱直接取水样10mL置于15mL固相微萃取瓶中，于40℃条件下固相微萃取吸附25min后，纤维头经风干，立即进样测定。该法对BDE-47和BDE-99的检出限分别为0.0000μg/L和0.0044μg/L，回归方程相关系数分别为0.9996和0.9992，RSD(n＝6)分别为6.7%～11

3、.4%和6.0%～10.1%。结果：随机抽样某市52个水样进行检测，均未检出BDE-47和BDE-99。结论：建立饮用水中多溴联苯醚固相萃取/固相微萃取-气相色谱检测的新方法，两种方法操作简便、快速，精密度、准确度及回收率均令人满意。关键词：固相萃取；固相微萃取；气相色谱；多溴联苯醚；饮用水DeterminationofPolybrominatedDiphenylEthersinDrinkingWaterbySolidPhaseExtractionorSolid-phaseMicro-extractio

4、nCombinedwithGasChromatographyHEYing-chun1，WANGZheng-hong2，LILin1,*，ZHOUQian-ru2(1.CollegeofFoodScience,SouthwestUniversity,Chongqing400716,China；2.ChongqingCenterforDiseasePreventionandControl,Chongqing400042,China)Abstract：Objective:Toestablishanovelme

5、thodfordeterminingthecontentsofpolybrominateddiphenylethers(BDE-47andBDE-99)indrinkingwaterbysolidphaseextraction(SPE)orsolidphasemicroextraction(SPME)combinedwithgaschromatography(GC).Methods:IntheSPE-GCmethod,100mLofwatersamplewaspurifiedbyLC-C18SPEcol

6、umnchromatographythroughelutionwithhexane.Theeluentwasevaporatedtodrynessinwaterbathat80℃,andtheremainingresiduewasre-dissolvedwithisooctaneandmadeupto1mL.Finally,1μLofthesolutionwasinjectedintoGCforthedetermination.Thelimitsofdetection(LOD)forBDE-47andB

7、DE-99were0.0008μg/Land0.0009μg/L(RSN=6),respectively,theregressionequationsshowedgoodlinearitywithacorrelationcoefficientof0.9996and0.9997,respectively,andtheRSDsfor6replicatedeterminationswereintherangeof1.0%－4.9%and0.96%－4.4%,respectively.IntheSPME-GCm

8、ethod,10mLofwatersamplewasplacedintoa15-mLSPMEbottleandadsorbedbysolid-phasemicro-extractionfor25minat40℃witharotationspeedof1150r/min.Then,thefiberwasair-dried,immediatelyfollowedbyGCanalysis.TheLODsoftheSPME-GCmethodforB