环境水样中卤代甲基磺酸的高效液相色谱-串联质谱联用分析方法研究

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英文篇名：Determination of five halogenated methyl sulfonic acids in environmental water by HPLC-MS/MS 作者：刘凯 ; 史亚利 ; 蔡亚岐 ; 何绪文 英文作者：LIU Kai;SHI Yali;CAI Yaqi;HE Xuwen;School of Chemical & Environmental Engineering,China University of Mining & Technology ( Beijing);State Key Laboratory of Environmental Chemistry and Ecotoxicology,Research Center for Eco-Environmental Science,Chinese Academy of Sciences; 关键词：卤代甲基磺酸 ; HPLC-MS/MS ; 固相萃取 英文关键词：halogenated methyl sulfonic acids;;HPLC-MS/MS;;solid phase extraction 中文刊名：环境化学 英文刊名：Environmental Chemistry 机构：中国矿业大学(北京)化学与环境工程学院;中国科学院生态环境研究中心环境化学与生态毒理学国家重点实验室; 出版日期：2018-12-18 14:55 出版单位：环境化学 年：2019 期：02 基金：国家水体污染控制与治理科技重大专项(2014ZX07405001)资助~~ 语种：中文; 页：44-50 页数：7 CN：11-1844/X ISSN：0254-6108 分类号：TU991.2

摘要

利用高效液相色谱三重四极杆串联质谱(HPLC-MS/MS),建立了环境水样中卤代甲基磺酸的分析方法.通过对固相萃取、色谱柱、流动相和质谱条件的优化,确定了最佳萃取和分析条件.选用WAX固相萃取柱对卤代甲基磺酸进行富集,再依次用2 m L的5%氨水甲醇溶液、2%甲酸甲醇溶液和20%二氯甲烷甲醇溶液(均为体积比)进行洗脱.选用Acclaim HILIC-10为色谱分离柱,以乙腈和100 mmol·L~(-1)甲酸铵水溶液为流动相,分离目标化合物,采用串联质谱负离子扫描和多反应监测模式进行检测.方法对5种卤代甲基磺酸(三氟甲基磺酸、一氯甲基磺酸、二氯甲基磺酸、三氯甲基磺酸和一溴甲基磺酸)的线性范围为0.05—50μg·L~(-1),线性相关系数r>0.99,各化合物的检出限(S/N=3)在0.005—0.039μg·L~(-1)之间.将建立的分析方法应用于实际样品中卤代甲基磺酸的测定,所得加标回收率在67.5%—95.4%之间,峰面积相对标准偏差(n=5)在8.5%—13.0%之间,可满足饮用水环境样品中痕量卤代甲基磺酸的分析.
        A method was developed for the determination of halogenated methyl sulfonic acids( HMSAs) in environmental water by solid phase extraction( SPE) coupled with high performance liquid chromatography-tandem mass spectrometry( HPLC-MS/MS). Parameters affecting the performance of SPE-LC-MS/MS were optimized,including SPE conditions,LC separation column and mass spectrometry parameters. A weak anion exchange( WAX) cartridge was chosen as the pretreatment column. After an environmental water sample was loaded into the WAX cartridge,the analytes were eluted using 2 m L of 5% ammonium hydroxide in methanol,2 m L of 2% formic acid in methanol,2 m L of the mixture solution with dichloromethane and methanol( 2 ∶ 8,V/V). Five HMSAs, including trifluoromethanesulfonic acid, chloromethanesulfonic acid, dichloromethanesulfonic acid, trichloromethanesulfonic acid, and bromomethanesulfonic acid, were separated on an Acclaim HILIC-10 column and detected using MS/MS with negative and multi reaction monitoring( MRM) mode. The mobile phase was mixture of acetonitrile( A) and100 mmol·L~(-1) ammonium formate solution( B) with pH at 6.5. Under the optimized conditions,the calibration range was from 0.05 to 50 μg·L~(-1). The method limits of detection( LOD) were in the range of 0.005—0.039 μg·L~(-1),which were calculated as the concentrations resulting in a signal-tonoise ratio at 3( S/N = 3). The developed method was successfully applied to HMSAs analysis in environmental water sample,with satisfied recoveries( 67. 5%—95. 4%) and relative standard deviations( RSD,n = 5) at 8.5%—13.0%.

引文

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