饮用水中5种新烟碱类杀虫剂的液相色谱质谱检测法

庄乾坤; 郑和辉; 卞战强; 田向红; 于建; 査玉娥; 张娟

doi:10.13421/j.cnki.hjwsxzz.2015.05.016

饮用水中5种新烟碱类杀虫剂的液相色谱质谱检测法

Simultaneous Determination of 5 Neonicotinoid Insecticides in Drinking Water by UPLC-MS

摘要

摘要:
目的建立直接进样同时检测饮用水中啶虫脒、噻虫啉、吡虫啉、烯啶虫胺和噻虫嗪5种新烟碱类杀虫剂残留的液相色谱串联质谱法。

方法水样经0.22μm滤膜过滤后,采用液相色谱柱分离,ESI正离子扫描多反应监测模式检测,外标法定量分析。色谱柱:Waters Acquity UPLC BEH C₁₈(2.1 mm×50 mm,1.7 μm)。

结果在2~200μg/L范围内5种杀虫剂所得回归方程的线性关系良好,相关系数均>0.99,检出限均<0.2μg/L,进行3个不同质量浓度的测定,每个浓度重复7次。该方法的平均回收率在88.5%~111.3%之间,相对标准偏差在0.8%~6.9%之间。

结论该方法操作简单、快速,准确度和灵敏度均能满足同时测定饮用水中多种新烟碱类杀虫剂残留的要求。

Abstract:
Objectives To establish a.Methods for simultaneous determination of 5 neonicotinoid insecticides, including acetamiprid, thiacloprid, imidacloprid, nitenpyram and thiamethoxam, in drinking water by liquid chromatography-tandem mass spectrometry.
Method After passing 0.22 μm filter membrane, water samples were injected directly to and detected by LC-MS. The chromatographic column was Waters Acquity UPLC BEH C₁₈(2.1 mm×50 mm,1.7 μm). The determination was performed at 3 levels, and each level was repeated for 7 times.
Results For all 5 neonicotinoid insecticides, a good linearity was in the range of 2~200 μg/L (r > 0.99); the limit of detection (LOD) was below 0.2 μg/L; the recovery rate for standard addition was in the range of 88.5%~111.3% and the relative standard deviation (RSD) was in the range of 0.8%~6.9%.
Conclusions The method was simple, fast, and its accuracy and sensitivity could be satisfied with simultaneous determination of 5 neonicotinoid insecticide residues in drinking water.

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