气相色谱-质谱联用法测定大气颗粒物PM_(10)中7种多溴二苯醚  

Determination of Polybrominated Diphenyl Ethers in Atmospheric Particulate Matter PM_(10) by Gas Chromatography-Mass Spectrometry

作　　者：李洒洒 王俊霞[1] 张一诺 沈诗洁 姜永波 王盼盼 张占恩[1,2,3] LI Sasa;WANG Junxia;ZHANG Yinuo;SHEN Shijie;JIANG Yongbo;WANG Panpan;ZHANG Zhanen(School of Environmental Science and Engineering,Suzhou University of Science and Technology,Suzhou 215009;Jiangsu Provincial Key Laboratory of Environmental Science and Engineering,Suzhou University of Science and Technology,Suzhou 215009;Innovation Center of Water Treatment Technology and Material:Suzhou University ofScience and Technology,Suzhou 215009)

机构地区：[1]苏州科技大学,环境科学与工程学院,江苏苏州215009 [2]苏州科技大学,江苏省环境科学与工程重点实验室,江苏苏州215009 [3]苏州科技大学,水处理技术与材料协同创新中心,江苏苏州215009

出　　处：《分析科学学报》2022年第5期605-610,共6页Journal of Analytical Science

基　　金：苏州科技计划项目(No.SNG2018050);江苏省环境科学与工程重点实验室开放课题(No.Zd1802);苏州科技大学2016年科研启动项目。

摘　　要：该研究优化了大气颗粒物PM_(10)中7种多溴二苯醚(PBDEs)提取及净化过程的实验条件,建立了气相色谱-质谱联用法(GC-MS)测定多溴二苯醚的方法。样品经正己烷-丙酮(1∶1,V/V)超声提取后,采用分散液-液微萃取进行净化富集,最后由GC-MS定量分析。7种多溴二苯醚的检出限为0.017-0.292 pg·m^(-3),定量下限为0.057-0.972 pg·m^(-3),加标回收率为72.77%-125.02%,相对标准偏差为0.42%-12.40%。该方法被用于苏州地区连续一周PM_(10)中PBDEs的测定,发现PBDEs同系物均被不同程度地检出。PM_(10)中7种∑PBDEs的检出浓度范围为0.241-0.678 ng·m^(-3)。In this study, the experimental conditions for the extraction and purification of 7 polybrominated diphenyl ethers(PBDEs) from atmospheric particulate matter PM_(10)were optimized, and the determination of PBDEs by gas chromatography-mass spectrometry(GC-MS)was established.The samples were ultrasonically extracted with n-hexane: acetone(1∶1,V/V),and then purified and enriched by dispersive liquid-liquid microextraction.Finally, it was quantitatively analyzed by gas chromatography-mass spectrometry.The limits of detection(LOD) was 0.017-0.292 pg·m^(-3),the limits of quantitation(LOQ) was 0.057-0.972 pg·m^(-3),the spiked recoveries ranged from 72.77% to 125.02%,and the RSDs ranged from 0.42% to 12.40%.This method was used for PBDEs determination of PM_(10)in Suzhou area for a week, and these results were shown some congener PBDEs were detected to certain extent in actual matrix.The detected concentrations of 7∑PBDEs in PM_(10)ranged from 0.241 to 0.678 ng·m^(-3).

关 键 词：分散液-液微萃取 超声提取 大气颗粒物 多溴二苯醚 气相色谱-质谱 

分 类 号：O657.63[理学—分析化学]