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超高效液相色谱串联质谱同时快速检测环境水体中31种内分泌干扰物

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黄文平, 胡霞林, 尹大强. 超高效液相色谱串联质谱同时快速检测环境水体中31种内分泌干扰物[J]. 环境化学, 2017, 36(4): 875-884. doi: 10.7524/j.issn.0254-6108.2017.04.2016101202
引用本文: 黄文平, 胡霞林, 尹大强. 超高效液相色谱串联质谱同时快速检测环境水体中31种内分泌干扰物[J]. 环境化学, 2017, 36(4): 875-884. doi: 10.7524/j.issn.0254-6108.2017.04.2016101202
shu
HUANG Wenping, HU Xialin, YIN Daqiang. Rapid and simultaneous determination of 31 endocrine disrupting chemicals in aquatic environment by ultra performance liquid chromatography-tandem mass spectrometry[J]. Environmental Chemistry, 2017, 36(4): 875-884. doi: 10.7524/j.issn.0254-6108.2017.04.2016101202
Citation: HUANG Wenping, HU Xialin, YIN Daqiang. Rapid and simultaneous determination of 31 endocrine disrupting chemicals in aquatic environment by ultra performance liquid chromatography-tandem mass spectrometry[J]. Environmental Chemistry, 2017, 36(4): 875-884. doi: 10.7524/j.issn.0254-6108.2017.04.2016101202
shu

超高效液相色谱串联质谱同时快速检测环境水体中31种内分泌干扰物

  • 1.

    同济大学环境科学与工程学院, 上海, 200092

  • 基金项目:

    国家自然科学基金（21277100，21577103）和水体污染控制与治理科技重大专项（2014ZX07402001）资助.

Rapid and simultaneous determination of 31 endocrine disrupting chemicals in aquatic environment by ultra performance liquid chromatography-tandem mass spectrometry

  • 1.

    College of Environmental Science and Engineering, Tongji University, Shanghai, 200092, China

  • Fund Project: Supported by the National Natural Science Foundation of China (21277100, 21577103) and Major Science and Technology Program for Water Pollution Control and Treatment (2014ZX07402001).

  • 摘要: 本文建立了固相萃取结合超高效液相色谱-串联质谱（SPE-UPLC-MS/MS）同时测定环境水体中31种内分泌干扰物（EDCs）的分析方法.水样通过MCX固相萃取柱一步富集.采用BEH C18色谱柱（150 mm×2.1 mm i.d.，1.7 μm）对化合物进行分离，0.025%氨水-甲醇梯度洗脱，电喷雾正负离子（ESI-、ESI+）两种电离模式切换、多反应监测（MRM）模式进行同时检测，内标法定量.31种EDCs在一定浓度范围内均呈良好的线性关系（R2≥0.99），方法检出限为0.01-3 ng·L-1.对Milli-Q纯水、自来水和地表水进行加标回收，日内、日间相对标准偏差值均小于25%.自来水和地表水样品的平均加标回收率分别为61.2%-150%、54.4%-141%和51.6%-127%、52.2%-143%.此方法一步固相萃取，31种物质同时检测，方便快捷，灵敏度高.该方法成功应用于饮用水和地表水（黄浦江和太湖）中31种EDCs的分析.
    Abstract: A method was developed for the simultaneous determination of 31 endocrine disrupting chemicals (EDCs) in environmental water by solid phase extraction combined with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Water samples were enriched by MCX solid-phase extraction columns in one step. The separation was performed on a BEH C18 column (150 mm×2.1 mm i.d.,1.7 μm) in gradient elution with methanol-0.025% ammonia aqueous solution as the mobile phase. The samples were detected by multiple reaction monitoring (MRM) mode with positive-negative electrospray ionization. Thirty one EDCs were quantified by internal standard method and the calibration curves showed good linearity in a wide range with correlation coefficients (R2) not less than 0.99. The detection limit of EDCs ranged from 0.01-3 ng·L-1. The average recovery of the 31 EDCs spiked in tap water and surface water samples ranged from 61.2%-150%, 54.4%-141% and 51.6%-127%, 52.2%-143% respectively. All the relative standard deviations of EDCs were less than 25%. The developed method is sensitive, convenient, rapid and reliable for the simultaneous determination of 31 EDCs in drinking water and surface water.
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  • 收稿日期:  2016-10-12
  • 刊出日期:  2017-04-15
黄文平, 胡霞林, 尹大强. 超高效液相色谱串联质谱同时快速检测环境水体中31种内分泌干扰物[J]. 环境化学, 2017, 36(4): 875-884. doi: 10.7524/j.issn.0254-6108.2017.04.2016101202
引用本文: 黄文平, 胡霞林, 尹大强. 超高效液相色谱串联质谱同时快速检测环境水体中31种内分泌干扰物[J]. 环境化学, 2017, 36(4): 875-884. doi: 10.7524/j.issn.0254-6108.2017.04.2016101202
shu
HUANG Wenping, HU Xialin, YIN Daqiang. Rapid and simultaneous determination of 31 endocrine disrupting chemicals in aquatic environment by ultra performance liquid chromatography-tandem mass spectrometry[J]. Environmental Chemistry, 2017, 36(4): 875-884. doi: 10.7524/j.issn.0254-6108.2017.04.2016101202
Citation: HUANG Wenping, HU Xialin, YIN Daqiang. Rapid and simultaneous determination of 31 endocrine disrupting chemicals in aquatic environment by ultra performance liquid chromatography-tandem mass spectrometry[J]. Environmental Chemistry, 2017, 36(4): 875-884. doi: 10.7524/j.issn.0254-6108.2017.04.2016101202
shu

超高效液相色谱串联质谱同时快速检测环境水体中31种内分泌干扰物

  • 1. 同济大学环境科学与工程学院, 上海, 200092
  • 收稿日期:  2016-10-12
基金项目:

国家自然科学基金（21277100，21577103）和水体污染控制与治理科技重大专项（2014ZX07402001）资助.

摘要: 本文建立了固相萃取结合超高效液相色谱-串联质谱（SPE-UPLC-MS/MS）同时测定环境水体中31种内分泌干扰物（EDCs）的分析方法.水样通过MCX固相萃取柱一步富集.采用BEH C18色谱柱（150 mm×2.1 mm i.d.，1.7 μm）对化合物进行分离，0.025%氨水-甲醇梯度洗脱，电喷雾正负离子（ESI-、ESI+）两种电离模式切换、多反应监测（MRM）模式进行同时检测，内标法定量.31种EDCs在一定浓度范围内均呈良好的线性关系（R2≥0.99），方法检出限为0.01-3 ng·L-1.对Milli-Q纯水、自来水和地表水进行加标回收，日内、日间相对标准偏差值均小于25%.自来水和地表水样品的平均加标回收率分别为61.2%-150%、54.4%-141%和51.6%-127%、52.2%-143%.此方法一步固相萃取，31种物质同时检测，方便快捷，灵敏度高.该方法成功应用于饮用水和地表水（黄浦江和太湖）中31种EDCs的分析.

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