MSPE-UPLC-MS/MS测定生活饮用水中呋喃丹、敌敌畏、乐果及马拉硫磷

Determination of Carbofuran, Dichlorvos, Dimethoate, and Malathion in Drinking Water by MSPE-UPLC-MS/MS

目的利用合成的磁性碳材料作吸附剂,建立一种快速测定生活饮用水中呋喃丹、敌敌畏、乐果及马拉硫磷4种农药残留量的磁分散固相萃取—超高效液相色谱串联质谱方法(MSPE-UPLC-MS/MS)。方法水样中加入磁性碳材料进行分散固相萃取,在外部磁场作用下弃去溶液后,加入甲醇洗脱,洗脱液过滤膜后经C;柱分离,电喷雾正离子化模式下,以多反应监测(multi-reaction monitoring, MRM)方式检测。结果呋喃丹、乐果和马拉硫磷在(0.10~50.0)μg/L,敌敌畏在(0.20~100.0)μg/L浓度范围内线性良好,分析物线性相关系数r≥0.999 0;方法检出限为(0.017~0.050)μg/L,最低检测质量浓度为(0.06~0.17)μg/L;3个浓度加标回收率为88.0%~105.7%范围内,相对标准偏差为2.0%~12.1%(n=6);磁性材料重复使用10次后依然具有较好的吸附性能。结论本方法简便、高效、准确,可用于生活饮用水中呋喃丹、敌敌畏、乐果及马拉硫磷4种农药残留量的检测。

Objective To establish a method for rapid determination of the residues of carbofuran, dichlorvos, dimethoate, and malathion in drinking water by magnetic dispersive solid-phase extraction combined with ultra-performance liquid chromatography-tandem mass spectrometry using synthesized magnetic carbon material as the adsorbent. Methods Magnetic carbon material was added to the drinking water sample for dispersive solid-phase extraction, and the solution was discarded under external magnetic field. Then methanol was used to desorb the analytes and the eluent was separated by a C;column after passing through the filter membrane and was detected by multiple reaction monitoring with electrospray ion source in positive ionization. Results Carbofuran, dimethoate, and malathion showed a good linear relationship within the range of(0.10-50.0)μg/L, and dichlorvos showed a good linear relationship within the range of(0.20-100.0)μg/L, with a correlation coefficient of 0.999 0 and above. The method had a limit of detection of(0.017-0.050)μg/L and a limit of determination of(0.06-0.17)μg/L. The average recovery at three spiking levels ranged from 88.0% to 105.7%, with a relative standard deviation of 2.0%-12.1%(n = 6). The magnetic material still had good adsorption performance after repeated use for 10 times. Conclusion This method is simple, efficient, and accurate and can be used to determine the residues of carbofuran, dichlorvos, dimethoate, and malathion in drinking water.