色谱

色谱 ›› 2018, Vol. 36 ›› Issue (9): 866-872.DOI: 10.3724/SP.J.1123.2018.04025

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱法快速测定地表水中联苯胺、苦味酸、甲萘威、阿特拉津和溴氰菊酯

张明1, 唐访良1, 徐建芬1, 张伟1, 程新良2, 王立群1   

  1. 1. 杭州市环境监测中心站, 浙江 杭州 310007;
    2. 淳安县环境保护监测站, 浙江 杭州 311700
  • 收稿日期:2018-04-23 出版日期:2018-09-08 发布日期:2014-08-05
  • 通讯作者: 唐访良,E-mail:TangFL001@163.com
  • 基金资助:

    杭州市社会发展科研攻关项目（20130533B02，20150533B08，20160533B84）.

Rapid determination of benzidine, picric acid, carbaryl, atrazine, and deltamethrin in surface water by ultra-performance liquid chromatography-tandem mass spectrometry

ZHANG Ming1, TANG Fangliang1, XU Jianfen1, ZHANG Wei1, CHENG Xinliang2, WANG Liqun1   

  1. 1. Hangzhou Environmental Monitoring Central Station, Hangzhou 310007, China;
    2. Chun'an Environmental Monitoring Station, Hangzhou 311700, China
  • Received:2018-04-23 Online:2018-09-08 Published:2014-08-05
  • Supported by:

    Scientific Research Fund for the Social Development of Hangzhou (Nos. 20130533B02, 20150533B08, 20160533B84).

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摘要：

建立了一种经简单过滤即可直接进样的超高效液相色谱-串联质谱（UPLC-MS/MS）分析方法，可快速测定地表水中联苯胺、苦味酸、甲萘威、阿特拉津和溴氰菊酯5种有机物的残留。样品经0.2 μ m针式滤头过滤除去颗粒性杂质后，进行UPLC-MS/MS分析，采用UPLC HSS T3色谱柱，2 mmol/L乙酸铵甲醇溶液和2 mmol/L乙酸铵水溶液作为流动相进行梯度洗脱，电喷雾离子源电离，正、负离子切换多反应监测模式进行定性和定量分析。5种目标化合物分别在0.10~10.0 μ g/L或1.00~100 μ g/L范围内线性关系良好，相关系数为0.996~0.999，方法的检出限为0.01~0.22 μ g/L；高、中、低3个添加水平的回收率为81.4%~113%，相对标准偏差为0.84%~14.0%。利用该方法对杭州市部分河流和水库的地表水样品进行分析，其中阿特拉津和溴氰菊酯在部分水样中有阳性检出。结果表明，该方法简便快捷、灵敏准确，适用于地表水样品中联苯胺、苦味酸、甲萘威、阿特拉津和溴氰菊酯的快速测定。

关键词: 阿特拉津, 超高效液相色谱-串联质谱, 甲萘威, 苦味酸, 联苯胺, 水, 溴氰菊酯

Abstract:

A method requiring no pre-treatment steps other than filtration, using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), has been developed and applied for the rapid determination of benzidine, picric acid, carbaryl, atrazine, and deltamethrin residues in surface water. Water samples were filtered with a 0.2-μ m syringe filter for particle removal and injected directly into the UPLC instrument. The separation was performed on a Waters Acquity UPLC HSS T3 column utilizing a gradient elution program of methanol (containing 2 mmol/L ammonium acetate) and water (containing 2 mmol/L ammonium acetate) as the mobile phases at a flow rate of 0.4 mL/min. The detection was accomplished by multiple-reaction monitoring scanning in positive/negative ion-switching electrospray ionization mode. Good linearity was observed in the range 0.10-10.0 μ g/L or 1.00-100 μ g/L for different targets with correlation coefficients of 0.996-0.999. The limits of detection (LODs) were 0.01-0.22 μ g/L. The recoveries ranged between 81.4% and 113% at three spiked levels with relative standard deviations (n=6) between 0.84% and 14.0%. The developed method was applied to the analysis of surface waters (river water and reservoir water) from Hangzhou; atrazine and deltamethrin were detected in part of the analyzed samples. This proposed method was characterized by high sensitivity and precision, extensive analytical range, and a high analytical rate, and showed suitability for the analysis of the five named pollutants in surface water.

Key words: atrazine, benzidine, carbaryl, deltamethrin, picric acid, ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), water

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