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微波萃取-气相色谱/质谱测定底泥中多溴联苯醚
引用本文:韩晓芳,陈亮,黄满红,陈东辉.微波萃取-气相色谱/质谱测定底泥中多溴联苯醚[J].环境科学与技术,2011,34(7):156-160.
作者姓名:韩晓芳  陈亮  黄满红  陈东辉
作者单位:东华大学环境科学与工程学院,上海,201620
基金项目:上海市科委项目(09230500200); 上海市重点学科建设项目资助(B604); 中央高校基本科研业务费专项基金(10D11308)
摘    要:文章建立微波萃取,复合硅胶氧化铝层析柱净化,气相色谱-负化学离子源质谱(GC-NCI-MS)检测对环境底泥样品中七种多溴联苯醚(PBDEs)单体定量分析的方法。底泥样品经25 mL正己烷:丙酮(1:1)萃取剂微波萃取10 min,过复合层析柱净化,70 mL正己烷:二氯甲烷(1:1)洗脱和浓缩后,加入内标物PCB-103后进行内标定量分析,7种PBDEs单体的平均基质加标回收率均值为88.6%~96.7%,相对标准偏差为1.9%~9.3%,方法检出限均小于0.06 ng/g,方法具有良好的重现性,较好的回收率和较高的灵敏度。所建立的分析方法体系已用于长江口近岸沉积物中7种PBDEs残留量的检测,四个实际样品中添加回收率指示物PCB-209,其回收率范围为79.5%~109.6%,相对标准偏差为5.2%~16.5%。

关 键 词:气相色谱-负化学离子源质谱  多溴联苯醚  沉积物  微波萃取  定量分析

Determination of Polybrominated Diphenyl Ethers in Sediments Using Microwave Extraction and GC-NCI-MS Spectrometry
HAN Xiao-fang,CHEN Liang,HUANG Man-hong,CHEN Dong-hui.Determination of Polybrominated Diphenyl Ethers in Sediments Using Microwave Extraction and GC-NCI-MS Spectrometry[J].Environmental Science and Technology,2011,34(7):156-160.
Authors:HAN Xiao-fang  CHEN Liang  HUANG Man-hong  CHEN Dong-hui
Institution:HAN Xiao-fang,CHEN Liang,HUANG Man-hong,CHEN Dong-hui(College of Environmental Science and Engineering,Donghua University,Shanghai 201620,China)
Abstract:Method of determination of polybrominated diphenyl ethers(PBDEs)contained in sediments is developed,which involves microwave extraction,multilayer silica and alumina column for clean-up and GC-NCI-MS for final determination. According to the experimental result,average recoveries of spiked samples range from 88.6 to 96.7%,with relative standard deviations between 1.9%and 9.3%,detection limit of the method being less than 0.06 ng/g.Besides,it is reported that a system based on this method has been applied to...
Keywords:GC-NCI-MS  polybrominated diphenyl ether(sPBDEs)  sediment  microwave extraction  quantitative analysis  
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