直接进样-超高效液相色谱串联质谱法同时测定生活饮用水中9种痕量氨基甲酸酯类农药的应用  

Simultaneous Determination of Nine Trace Carbamate Pesticides in Drinking Wate by UPLC-MS/MS With Direct Injection

作　　者：江阳[1] 王艳[1] 杨丰义 孙成均[2] 周定友[1] 金伟[1] 雍莉[1] 胡彬[1] JIANG Yang;WANG Yan;YANG Fengyi;SUN Chengjun;ZHOU Dingyou;JIN Wei;YONG Li;HU Bin(Sichuan Center for Disease Control and Prevention,Chengdu 610041,Sichuan Province,China;West China School of Public Health,Sichuan University,Chengdu 610041,Sichuan Province,China)

机构地区：[1]四川省疾病预防控制中心,成都610041 [2]四川大学华西公共卫生学院,成都610041

出　　处：《预防医学情报杂志》2019年第5期498-504,共7页Journal of Preventive Medicine Information

摘　　要：目的建立同时测定饮用水中9种痕量氨基甲酸酯类农药(速灭威、异丙威、甲萘威、猛杀威、涕灭威、呋喃丹、三羟基克百威、抗蚜威、硫双威)残留的直接进样-超高效液相色谱串联质谱方法。方法水样经0.22μm的滤膜过滤后,通过UPLC-MS/MS分析测定,色谱柱采用Acquity UPLC BEH C18柱(2.1 mm×100 mm,1.7μm),以甲醇-0.05%酸水溶液为流动相,梯度洗脱。采用电喷雾电离(ESI),多反应监测(MRM)模式进行检测,外标法定量。结果 9种氨基甲酸酯类农药在0.10μg/L～10μg/L范围内具有良好的线性关系,相关系数均大于0.998 8。加标回收率为81.3%～111.0%,相对标准偏差为1.25%～10.0%,方法检出限为0.002μg/L～0.015μg/L,定量限为0.005μg/L～0.05μg/L。结论该法简便快速、灵敏度高,适用于生活饮用水中9种痕量氨基甲酸酯类农药的批量测定。Objective To establish a method for the simultaneous determination of nine carbamate pesticides including metol carb,isoprocorb, carbaryl, 3-hydroxycarbofuran, promecrab, aldicarb,carbofuran, thiodicarb and pirimicarb in drinking water using ultra performance liquid chromatography tandem mass spectrometry with direct injection. Methods Water samples were filtrated with a 0.22 μm millipore filter, then detected by HPLC-MS/MS. The analytes were separated on a Acquity UPLC BEH C18 column(2.1 mm × 100 mm, 1.7 μm) using a programmed gradient elution with a mobile phase consisting of methanol,water and formic acid, electrospray ionization(ESI) and multi-reaction monitoring(MRM) were used for the detection. The quantification was based on the external standard calibration curves. Results Good linearities were obtained in the range of 0.1 μg/L to 10 μg/L for the nine carbamate pesticides, each with correlation coefficient larger than 0.998 8. The detection limits were from 0.002 μg/L to 0.015 μg/L,while the quantification limits were from 0.005 μg/L to0.05 μg/L, the average recoveries were from 81.3% to 111.0% with relative standard deviations(RSDs) of 1.25%~10.0%. Conclusion The established method is simple, sensitive, and can accurately determine nine trace carbamate pesticides in drinking water.

关 键 词：直接进样 HPLC-MS/MS 氨基甲酸酯类农药 饮用水 

分 类 号：R123.1[医药卫生—环境卫生学]