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

作　　者：杨雪丽 王猛 李菁[1] 马鑫[1] 付慧[2] 丁昌明[2] YANG Xueli;WANG Meng;LI Jing;MA Xin;FU Hui;DING Changming

机构地区：[1]新疆自治区疾病预防控制中心卫生监测检验中心,新疆维吾尔自治区乌鲁木齐市830001 [2]中国疾病预防控制中心环境与健康相关产品安全所

出　　处：《环境卫生学杂志》2020年第2期201-206,共6页JOURNAL OF ENVIRONMENTAL HYGIENE

基　　金：新疆维吾尔自治区卫生计生委青年医学科技人才专项(wjwy-2018011)。

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0.22μm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,1.7μm)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。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 0.22μm 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,1.7μm).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 were91.5%~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.

关 键 词：呋喃丹 有机磷 超高效液相色谱串联质谱 生活饮用水 

分 类 号：R123.1[医药卫生—环境卫生学]