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固相萃取-气相色谱串联质谱法同时测定水中多种农药

Solid-phase extraction and gas chromatography-tandem mass spectrometry method for the simultaneous determination of several pesticides in water.

机构信息

Laboratório Central, Empresa Portuguesa das Aguas Livres, S.A., EPAL, Rua do Alviela 12, 1170-012 Lisboa, Portugal.

出版信息

Water Sci Technol. 2010;62(3):667-75. doi: 10.2166/wst.2010.915.

Abstract

Contamination of surface and groundwater sources with pesticide residues has been of great concern for a long time and it is a major challenge for the preservation and sustainability of the environment. In order to accomplish the requirements of the European Directive 98/83/EC, we developed and validated an analytical method based on the combination of gas chromatography and tandem quadrupole mass spectrometry (GC-MS/MS) using solid-phase extraction as sample preparation. In this work nine pesticides were studied: molinate, simazine, atrazine, terbuthylazine, diazinon, alachlor, metalaxyl, metolachlor and pendimethalin. In order to get the best sensitivity and selectivity for each pesticide, several parameters of the tandem mass spectrometry were optimized using the MRM mode. Good linearity of the detector response was found for all pesticides at concentrations within the tested working range, with linear determination coefficients higher than 0.9988. Recoveries studies in several matrices with different fortification levels were performed, with recoveries between 77 and 115% with RSD lower than 9.5%. The MQLs obtained for these compounds were between 0.013 microg L(-1) and 0.022 microg L(-1), which were much lower than the maximum level established by the European legislation.

摘要

长期以来,地表和地下水源受到农药残留污染一直是人们关注的焦点,这也是环境保护和可持续性的主要挑战。为了满足欧洲指令 98/83/EC 的要求,我们开发并验证了一种基于固相萃取作为样品制备的气相色谱-串联四极杆质谱联用(GC-MS/MS)分析方法。在这项工作中,研究了 9 种农药:灭草磷、西玛津、莠去津、特丁津、二嗪磷、甲草胺、金属axyl、甲霜灵和二甲戊灵。为了获得每种农药的最佳灵敏度和选择性,使用 MRM 模式优化了串联质谱的几个参数。所有农药在测试工作范围内的浓度均表现出良好的线性响应,线性测定系数均高于 0.9988。在不同加标水平的多种基质中进行了回收率研究,回收率在 77%至 115%之间,相对标准偏差(RSD)低于 9.5%。这些化合物的 MQL 介于 0.013 微克/升至 0.022 微克/升之间,远低于欧洲法规规定的最高水平。

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