同位素稀释/高分辨气相色谱-质谱联用同时测定空气中二英、多氯联苯、多溴联苯醚和溴代二英

Simultaneous Determination of Polychlorinated Dibenzo-p-Dioxins/Furans,Polybrominated Dibenzo-p-Dioxins/Furans,Polychlorinated Biphenyls and Polybrominated Diphenyl Ethers by Isotope Dilution-High Resolution Gas Chromatography-High Resolution Mass Spectrom

建立了一套全自动索氏萃取仪,采用快速提取-酸性硅胶层析柱-酸碱多层硅胶层析柱-活性炭分散硅胶柱-同位素稀释/高分辨气相色谱-质谱联用分析技术同时测定环境空气中二噁英、多氯联苯、多溴联苯醚和溴代二噁英类化合物。利用淋洗曲线片段切割技术消除了多氯联苯和多溴联苯醚的空白干扰,优化了样品提取及前处理方法。在优化条件下,对环境空气进行测定,采样内标回收率范围在63%～100%之间、净化内标在52%～132%之间,方法检出限在6×10-4～1×10-2pg/m3之间,其中BDE-209的检出限为0.3pg/m3,满足环境空气中4类化合物的分析要求。二噁英和二噁英类多氯联苯毒性当量和在0.216～0.949pg/m3（WHO-TEQ）之间,溴代二噁英毒性当量为0.0181～0.0462pg/m3（WHO-TEQ）,多溴联苯醚含量范围为105～132pg/m3。

A method for simultaneous determination of polychlorinated dibenzo-p-dioxins/furan （PCDD/Fs）, polybrominated dibenzo-p-dioxins/furans （PBDD/Fs） , polyehlorinated biphenyls （PCBs） and polybrominated diphenyl ethers （PBDEs） was established by using elution curve and fraction cut technology to eliminate the PCB and PBDE blank of interference and optimize the pre-treatment. The technology was developed using AutoSoxtec, acid silica gel column, multi-layered silica gel column and active carbon column. The sample recovery of sampling standards was in the range of 63%-100% and the recovery of internal standards was in the range of 52%-132%. The detection limits was between 6×10-4-1×10-2 pg/mz, dicabromodiphenyl ether （ BDE-209 ） was 0.3 pg/m3, which reached the US Environmental Protection Agency （EPA） standards. Air sample toxic equivalent quantity （TEQ） （PCDD/Fs, dl-PCBs） was between 0. 216-0. 949 pg/L WHO-TEQ, TEQ（PBDD/Fs） was 0. 0181-0. 0462 pg/L WHO-TEQ, and PBDEs content was 105-132 pg/m3.