饮用水中8种有机磷类农药和除草剂及氨基甲酸酯类农药的超高效液相色谱-串联质谱直接测定法

Simultaneous determination of eight kinds of organophosphorus pesticides,urethane pesticides and herbicide in drinking water by direct injection ultra-performance liquid chromatography tandem mass spectrometry

目的建立饮用水中8种有机磷类农药、氨基甲酸酯类农药和除草剂的超高效液相色谱-串联质谱直接测定法。方法水样经离心、0.22μm滤膜过滤后,以Eclipse Plus C18色谱柱（50 mm×2.1 mm,1.8μm）为分析柱,甲醇和0.1%甲酸水为流动相,采用正离子动态多离子反应监测模式检测。结果在1.00~100.00μg/L的浓度范围内,所得8种农药的标准曲线线性关系良好,r为0.999 1~0.999 9。该方法对8种农药的检出限分别为0.002~0.08μg/L,定量下限分别为0.005~0.25μg/L;加标回收率为91.9%~102.8%,RSD为1.1%~6.8%。结论该方法样品前处理简单、快捷,且灵敏度高、精密度和准确度好、定性能力强,能更好地适应复杂水样中多组分的检测。

Objective To establish a direct injection ultra-performance liquid chromatography tandem mass spectrometry method for the determination of eight kinds of organophosphorus pesticides,urethane pesticides and herbicide in drinking water.Methods The water samples were filtered by centrifugation and 0.22 μm membrane, and directly analyzed by UPLC-MS/MS using Eclipse Plus C18 column（50 mm×2.1 mm,1.8 μm） in dynamic multiple reaction monitoring（Dynamic MRM） acquisition under positive ion mode. The mobile phase was 0.1% formic acid and methanol. Results In the linear range of 1.00-100.00μg/L, the regression equation of the eight kinds of organophosphorus pesticides,urethane pesticides and herbicide showed good linear relationship, r=0.999 1-0.999 9. The limit of detection was between 0.002 and 0.08 μg/L, the quantification limit of the method was between 0.005 and 0.25 μg/L, the average recovery rates were between 91.9% and 102.8%, and the RSDs were between 1.1% and 6.8%. Conclusion The method is simple,rapid,sensitive, accurate and applicable to the determination of multi-components in pesticides in drinking water.