超高效液相色谱串联质谱法测定饮用水中呋喃丹及5种有机磷农药

杨雪丽; 王猛; 李菁; 马鑫; 付慧; 丁昌明

doi:10.13421/j.cnki.hjwsxzz.2020.02.021

超高效液相色谱串联质谱法测定饮用水中呋喃丹及5种有机磷农药

Determination of Carbofuran and Five Organophosphorus Pesticides Simultaneously in Drinking Water by Ultra Performance Liquid Chromatography-Electrospray Tandem Mass Spectrometry

摘要

摘要:
目的建立直接测定生活饮用水中乐果、敌敌畏、甲基对硫磷、马拉硫磷、毒死蜱、呋喃丹6种常用农药的超高效液相色谱串联质谱（UPLC-MS/MS）分析方法。
方法样品按水样:甲醇=1:1比例混合后，经0.22 μm聚四氟乙烯（PTFE）滤膜过滤后直接进样，采用ACQUITY UPLC BETH C₁₈（100 mm×2.1 mm，1.7 μm）分析柱，以乙腈和0.1%甲酸水溶液为流动相，进行梯度淋洗。在电喷雾正离子模式（ESI+）下电离，多反应监测模式（MRM）进行检测，外标法定量。
结果乐果、敌敌畏、马拉硫磷、毒死蜱、呋喃丹在（0.5~100）μg/L，甲基对硫磷在（2.0~400）μg/L浓度范围内，线性关系良好（r≥0.999），方法检出限为（0.05~0.26）μg/L，平均回收率为91.5%~107.4%，相对标准偏差（RSD）1.4%~7.1%。
结论该方法前处理简单、高效、准确、灵敏度高、选择性好，适用于生活饮用水中上述6种农药的测定。

Abstract:
Objective An ultra performance liquid chromatography-electrospray tandem mass spectrometry (UPLC-MS/MS) method was established for the simultaneous determination of dimethoate, dichlorvos, methyl parathion, malathion, chlorpyrifos and carbofuran, in drinking water.
Methods The water samples was filtrated with 0.22 μm PTFE millipore filter after dilutin with methanol-water 1:1, and then injected and detected directly by UPLC-MS/MS. Chromatographic column used for separation was ACQUITY UPLC BETH C₁₈(100 mm×2.1 mm, 1.7 μm). Acetonitrile -water-0.1% formic acid was used as the mobile phase to conduct gradient elution. Identification was achieved by electrospray ionization(ESI+) in multiple reaction monitoring modes. Quantification was performed by the external standard calibration.
Results The calibration curves of 6 pesticides showed good linearity in suitable ranges with correlation coefficient (r) over 0.9990. The detection limits were in the range of(0.05~0.26)μg/L. The recoveries of standard addition were 91.5%~107.4%, and the RSDs were 1.4%~7.1%.
Conclusion The method is simple, rapid, sensitive and suitable for simultaneous determination of six pesticides in drinking water.

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