色谱

色谱 ›› 2018, Vol. 36 ›› Issue (10): 1018-1021.DOI: 10.3724/SP.J.1123.2018.06031

• 研究论文 • 上一篇    下一篇

在线固相萃取-超高效液相色谱-串联质谱法快速测定地表水中超痕量阿特拉津

沈斐1,2, 许燕娟1, 宋挺1, 陈静1, 王晔1   

  1. 1. 无锡市环境监测中心站, 江苏 无锡 214121;
    2. 江南大学环境与土木工程学院, 江苏 无锡 214122
  • 收稿日期:2018-06-28 出版日期:2018-10-08 发布日期:2014-08-22
  • 通讯作者: 沈斐,E-mail:feirenlei911@aliyun.com
  • 基金资助:

    江苏省环境监测科研基金项目（1612）；无锡市社会发展科技示范工程项目（CSE12N1603）.

Rapid determination of ultra-trace levels of atrazine in surface water by on line solid phase extraction coupled with ultra-performance liquid chromatography-tandem mass spectrometry

SHEN Fei1,2, XU Yanjuan1, SONG Ting1, CHEN Jing1, WANG Ye1   

  1. 1. Wuxi Environmental Monitoring Central Station, Wuxi 214121, China;
    2. School of Environment and Civil Engineering, Jiangnan University, Wuxi 214122, China
  • Received:2018-06-28 Online:2018-10-08 Published:2014-08-22
  • Supported by:

    Environmental Monitoring and Research Foundation of Jiangsu Province (No. 1612); Wuxi Social Development Science and Technology Demonstration Project (No. CSE12N1603).

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摘要：

建立了在线固相萃取-超高效液相色谱-串联质谱（on line SPE-UPLC-MS/MS）测定地表水中超痕量阿特拉津的方法。样品经滤膜过滤，HLB Direct Connect HP在线固相萃取小柱富集纯化，甲醇溶液洗脱，以Acquity BEH 130为分析柱，串联质谱进行检测，外标法定量。阿特拉津在1.0~5000 ng/L范围内线性关系良好，相关系数（r）为0.9989；该方法检出限为0.2 ng/L，阿特拉津的回收率为83.0%~105.1%，相对标准偏差为1.6%~5.3%（n=7），满足超痕量分析测试的要求。该法灵敏度高，分析速度快，对于保障水环境安全、及时提供污染信息、有效应对环境应急突发事件具有十分重要的意义。

关键词: 阿特拉津, 超高效液相色谱-串联质谱, 超痕量, 地表水, 在线固相萃取

Abstract:

A method for the determination of ultra-trace atrazine in surface water was developed based on on line solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (on line SPE-UPLC-MS/MS). The water sample was directly injected into an on line SPE system after filtering using a 0.22 μm filter membrane. An HLB Direct Connect HP column was used for the enrichment and purification of the water sample and eluted using a methanol solution. The analyte was separated on an Acquity BEH 130 column, and then detected by tandem mass spectrometry. The analyte was quantified with external standard method. There was a good linear relationship in the range of 1.0-5000 ng/L. The correlation coefficient (r) was 0.9989. The method detection limit was 0.2 ng/L. The recoveries of atrazine ranged from 83.0% to 105.1%. The relative standard deviation was 1.6%-5.3% (n=7), which met the requirements of trace analysis. The method is sensitive, fast and effective, and it is suitable for the determination of atrazine in surface water. It is important to ensure the safety of the water environment, provide timely pollution information, and effectively respond to environmental emergencies.

Key words: atrazine, on line solid phase extraction (on line-SPE), surface water, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), ultra-trace levels

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