摘要
目的建立水中9种新烟碱类农药的直接进样-高效液相色谱-串联质谱(HPLC-MS/MS)分析方法。方法水样经0.22μm滤膜过滤后直接进样,经色谱柱Accucore aQ(100×2.1 mm,2.6μm)分离,以甲醇-0.05%甲酸水(水相含2 mM甲酸铵)为流动相进行梯度洗脱,采用电喷雾电离源(ESI)、多反应监测(MRM)模式检测,内标法定量。采用Excel 2016软件进行数据描述性分析。结果9种新烟碱类农药在0.10~10.0μg/L范围内有良好的线性关系(r>0.9993),方法的检出限在0.0006~0.0150μg/L之间,方法的定量限在0.002~0.050μg/L之间;回收率在90.5%~101.3%范围内,相对标准偏差为1.3%~5.0%。结论本研究建立的直接进样-高效液相色谱-串联质谱法前处理简便,灵敏度高、重现性好,适用于生活饮用水中9种新烟碱类农药的同时快速检测。
Objective To develop a direct injection-high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method for the determination of nine neonicotinoid pesticides in drinking water.Methods The water samples were filtered by 0.22μm filter membranes and then injected and detected directly by HPLC-MS/MS.The analytes were separated on an Accucore aQ column(100×2.1 mm,2.6μm)by using a programmed gradient elution with a mobile phase consisting of methanol and 0.05%formic acid water with 2 mM ammonium formate,and detected by electrospray ionization(ESI)in multiple reaction monitoring(MRM)mode.The quantification was performed by the internal standard calibration method.Results The linear range of nine analytes ranged from 0.10μg/L to 10.0μg/L(r>0.9993),the detection limit of the method was betweeen0.0006-0.0150μg/L,and the quantitative limit was between 0.002-0.050μg/L.The recoveries were90.5%-101.3%with relative standard deviations(RSDs)of 1.3%-5.0%.Conclusions The method of direct injection high performance liquid chromatography-tandem mass spectrometry can accurately determine nine neonicotinoid pesticides in drinking water,with simple preptreatment,high sensitivity and excellent repeatability.
作者
江阳
陈雨露
赵咏梅
金伟
董思敏
雍莉
李永新
JIANG Yang;CHEN Yulu;ZHAO Yongmei;JIN Wei;DONG Simin;YONG Li;LI Yongxin(Sichuan Provincial Center for Disease Control and Prevention,Chengdu 610041,Sichuan Province,China;West China School of Public Health(West China Fourth Hospital),Sichuan University,Chengdu 610041,Sichuan Province,China.)
出处
《预防医学情报杂志》
CAS
2023年第12期1513-1519,共7页
Journal of Preventive Medicine Information
