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在线固相萃取-超高效液相色谱法检测水中14种有机磷酸酯

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张恒, 郭昌胜, 吕佳佩, 裴莹莹, 殷行行, 高建峰, 徐建. 在线固相萃取-超高效液相色谱法检测水中14种有机磷酸酯[J]. 环境化学, 2020, (4): 1047-1054. doi: 10.7524/j.issn.0254-6108.2019103005
引用本文: 张恒, 郭昌胜, 吕佳佩, 裴莹莹, 殷行行, 高建峰, 徐建. 在线固相萃取-超高效液相色谱法检测水中14种有机磷酸酯[J]. 环境化学, 2020, (4): 1047-1054. doi: 10.7524/j.issn.0254-6108.2019103005
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ZHANG Heng, GUO Changsheng, LYU Jiapei, PEI Yingying, YIN Xingxing, GAO Jianfeng, XU Jian. Determination of 14 organic phosphate esters in water by high performance liquid chromatography coupled with online solid phase extraction[J]. Environmental Chemistry, 2020, (4): 1047-1054. doi: 10.7524/j.issn.0254-6108.2019103005
Citation: ZHANG Heng, GUO Changsheng, LYU Jiapei, PEI Yingying, YIN Xingxing, GAO Jianfeng, XU Jian. Determination of 14 organic phosphate esters in water by high performance liquid chromatography coupled with online solid phase extraction[J]. Environmental Chemistry, 2020, (4): 1047-1054. doi: 10.7524/j.issn.0254-6108.2019103005
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在线固相萃取-超高效液相色谱法检测水中14种有机磷酸酯

  • 1. 中北大学理学院, 太原, 030051;

  • 2. 中国环境科学研究院环境健康风险评估与研究中心, 北京, 100012;

  • 3. 环境基准与风险评估国家重点实验室, 北京, 100012;

  • 4. 国家环境保护化学品生态效应与风险评估重点实验室, 北京, 100012

    • 通讯作者: 郭昌胜, E-mail: guocs@craes.org.cn ; 
  • 基金项目:

    国家水体污染控制与治理科技重大专项（2017ZX07301005-003，2017ZX07302001）和国家自然科学基金（41673120）资助.

Determination of 14 organic phosphate esters in water by high performance liquid chromatography coupled with online solid phase extraction

  • 1. College of Science, North University of China, Taiyuan, 030051, China;

  • 2. Center for Environmental Health Risk Assessment and Research, Chinese Research Academy of Environmental Sciences, Beijing, 100012, China;

  • 3. State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing, 100012, China;

  • 4. State Environmental Protection Key Laboratory of Ecological Effect and Risk Assessment of Chemicals, Chinese Research Academy of Environmental Sciences, Beijing, 100012, China

    • Corresponding author: GUO Changsheng, guocs@craes.org.cn ; 
  • Fund Project: Supported by the National Water Pollution Control and Management Science and Technology Major Project (2017ZX07301005-003, 2017ZX07302001) and the National Natural Science Foundation of China (41673120).

  • 摘要: 与传统固相萃取耗时长、工作量大、有机溶剂使用量多相比，本文建立了一种在线固相萃取-超高效液相色谱串联质谱方法同时测定地表水中14种有机磷酸酯的新方法.地表水样过膜后，直接注入在线固相萃取净化装置，经净化后进入分离柱分离，用乙腈和0.1%的甲酸水溶液梯度洗脱，采用电喷雾离子源正离子多反应监测模式，对14种有机磷酸酯类化合物进行检测，内标法定量.该方法分析时长13.0 min，方法的线性相关系数R2>0.98，地表水和自来水样品的加标回收率在64.8%—113%，相对标准偏差RSD在1.2%—9.3%，检出限为0.1—2.7 ng·L-1.与常规方法相比，该方法提高了分析通量和灵敏度，准确度好，操作简便，适用于地表水和自来水中有机磷酸酯的检测.
    Abstract: Compared with conventional solid phase extraction method which is time-consuming, low efficiency, large workload and large amount of organic solvent needed, this study established a new online solid phase extraction -ultra high performance liquid chromatography-tandem mass spectrometry method for simultaneous determination of 14 organic phosphate esters in surface water. After passing through the membrane filter, the surface water sample was directly injected into the on-line solid phase extraction purification device. After purification, samples were separated in the separation column, and the gradient was eluted with acetonitrile and 0.1% formic acid aqueous solution. The electrospray ion source positive ion multi-reaction monitoring mode was used to detect the organophosphate ester compounds. The total analysis time of this method was 13.0 min, the linear correlation coefficient of the method R2 was greater than 0.98, the spiked recovery of surface water and tap water samples was between 64.8%—113%, and the relative standard deviation RSD was between 1.2%—9.3%. The detection limit was between 0.1 and 2.7 ng·L-1. Compared with the conventional method, the online SPE method was suitable for detecting organic phosphate esters in surface water and tap water with high analysis flux and sensitivity, good accuracy and easy to operate.
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  • 收稿日期:  2019-10-30

在线固相萃取-超高效液相色谱法检测水中14种有机磷酸酯

    通讯作者: 郭昌胜, E-mail: guocs@craes.org.cn ; 
  • 1. 中北大学理学院, 太原, 030051;
  • 2. 中国环境科学研究院环境健康风险评估与研究中心, 北京, 100012;
  • 3. 环境基准与风险评估国家重点实验室, 北京, 100012;
  • 4. 国家环境保护化学品生态效应与风险评估重点实验室, 北京, 100012
  • 收稿日期:  2019-10-30
基金项目:

国家水体污染控制与治理科技重大专项（2017ZX07301005-003，2017ZX07302001）和国家自然科学基金（41673120）资助.

摘要: 与传统固相萃取耗时长、工作量大、有机溶剂使用量多相比，本文建立了一种在线固相萃取-超高效液相色谱串联质谱方法同时测定地表水中14种有机磷酸酯的新方法.地表水样过膜后，直接注入在线固相萃取净化装置，经净化后进入分离柱分离，用乙腈和0.1%的甲酸水溶液梯度洗脱，采用电喷雾离子源正离子多反应监测模式，对14种有机磷酸酯类化合物进行检测，内标法定量.该方法分析时长13.0 min，方法的线性相关系数R2>0.98，地表水和自来水样品的加标回收率在64.8%—113%，相对标准偏差RSD在1.2%—9.3%，检出限为0.1—2.7 ng·L-1.与常规方法相比，该方法提高了分析通量和灵敏度，准确度好，操作简便，适用于地表水和自来水中有机磷酸酯的检测.

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