高分辨气相色谱-质谱法同时测定土壤及沉积物中二英、溴代二英、多氯联苯和多溴联苯醚  

Simultaneous deiermination of PCDD /Fs,PBDD /Fs,DL-PCBs and PBDEs with high rosolution gas chromatography-mass spectrometry in soil and sediment samples

作　　者：朱国华[1] 巩宏平[1] 邵科[1] 高丹[2] 周欣[1] 王玲[1] 刘劲松[1] 

机构地区：[1]浙江省环境监测中心,杭州310015 [2]浙江工业大学,杭州310014

出　　处：《环境化学》2014年第1期74-80,共7页Environmental Chemistry

基　　金：浙江省重大科技专项(2009C13004);国家高技术研究发展计划(863计划)项目(2011AA060604);浙江省环保科技项目(2012A038)资助

摘　　要：采用同位素内标稀释-高分辨气相色谱-高分辨质谱法同时测定土壤及沉积物样品中PCDD/Fs、PBDD/Fs、DL-PCBs和PBDEs 4种二英类持久性有机物的含量.利用凝胶渗透色谱、多层酸碱硅胶净化柱、活性炭分散硅胶净化柱针对不同二英类污染物的不同吸附特性,运用不同极性的溶剂淋洗,实现二英组分(PCDD/Fs、PBDD/Fs)和其他两个组分(DL-PCBs、PBDEs)的分离,排除了同系物间及其他物质的干扰.所建方法的精密度变化范围在1.4%—13.6%之间,净化内标回收率范围在61%—104%之间,PCDD/Fs和PBDD/Fs的检出限分别在0.048—0.153 pg·g-1和0.044—0.395 pg·g-1之间,DL-PCBs和PBDEs的检出限分别在0.028—0.105 pg·g-1和0.034—10.2 pg·g-1之间,目标物检测结果大部分在质控样品标准范围之内,本文所建立的方法可以用于土壤及沉积物中PCDD/Fs、PBDD/Fs、DL-PCBs和PBDEs的同时净化分离.A method for simultaneous determination of PCDD/Fs （polybrominateddibenzo-p-dioxins and dibenzo-furans）, PBDD/Fs （polychlorinated dibenzo-p-dioxins and dibenzo-furans）、DL-PCBs （Dioxin-Like polychlorinated biphenyls） and PBDEs （diphenyl ethers） by isotope dilution-HRGC-MS（high resolution gas chromatography-mass spectrometry） was established based on the USEPA standard methods numbered as 1613B,1614,1668A and previous studies. Gel permeation chromatography,multi-layered silica gel and active carbon column were used in the comprehensive procedure. Due to the differences in planarity and adsorption properties,dioxin components（PCDD/Fs,PBDD/Fs） were separated from the other two groups （DL-PCBs,PBDEs） with different polarity solvent elution and isomers or others disturbances were excluded well. Under optimum conditions,precision was in the range of 1.4%—13.6%,the spiked recovery was in the range of 76%—111%,and the limit of detection （LOD） for PCDD/Fs,PBDD/Fs,DL-PCBs and PBDEs was in the range of 0.048—0.153 pg·g-1,0.044—0.395 pg·g-1,0.028—0.105 pg·g-1,0.034—10.2 pg·g-1 respectively.The results showed that the method allowed the reliable investigation of soil and sediment samples.

关 键 词：二英 同位素稀释法 高分辨磁质谱 串联质谱 

分 类 号：X833[环境科学与工程—环境工程] O657.63[理学—分析化学]