Luo Xiaofei, Wu Ling, Sun Chengjun, Yang Xiaosong, Wen Jun, Ye Qian, Zhang Jing
Chengdu Center for Disease Control and Prevention, Chengdu 610041, China.
West China School of Public Health, Sichuan University, Chengdu 610041, China.
Wei Sheng Yan Jiu. 2019 Jan;48(1):120-128.
To develop a method for the simultaneous determination of 67 pesticides in water by solid phase extration(SPE) disk extraction-gas chromatography-tandem mass spectrometry(GC-MS/MS).
Pesticides in water were extracted and cleaned-up with SPE disk, then eluted with dichloromethane-n-ethyl acetate(7∶3, V/V). After the eluent being concentrated to 1 mL under nitrogen blow at 40 ℃, the supernatant was injected into GC-MS/MS for analysis. The GC separation was performed on a DB-5 MS capillary column(30 m×0. 25 mm×0. 25 μm). The pesticides were detected by MS/MS in multiple reaction monitoring(MRM) mode and quantified by working curve method.
The linear range of the method for most of the pesticides were in the range of 0. 05-5 μg/L with correlation coefficients of 0. 9924-0. 9999. The quantitative limits(S/N=10) of the method were in the range of 1. 0×10~(-5)-0. 059 μg/L. The recoveries for pesticides were 81. 0%-125. 0% with relative standard deviations of 1. 5%-21. 4%(n=6).
The method is sensitive, simple, environmentally friendly and suitable to the determination of pesticides in drinking water for rapid screening and quantitative analysis.
建立一种采用固相萃取（SPE）圆盘萃取-气相色谱-串联质谱法（GC-MS/MS）同时测定水中67种农药的方法。
水中农药用SPE圆盘萃取并净化，然后用二氯甲烷-乙酸乙酯（7∶3，V/V）洗脱。洗脱液在40℃氮吹浓缩至1 mL后，取上清液注入GC-MS/MS进行分析。GC分离在DB-5 MS毛细管柱（30 m×0.25 mm×0.25μm）上进行。农药采用多反应监测（MRM）模式的MS/MS检测，工作曲线法定量。
该方法对大多数农药的线性范围为0.05 - 5μg/L，相关系数为0.9924 - 0.9999。方法的定量限（S/N = 10）为1.0×10⁻⁵ - 0.059μg/L。农药回收率为81.0% - 125.0%，相对标准偏差为1.5% - 21.4%（n = 6）。
该方法灵敏、简便、环保，适用于饮用水中农药的快速筛查和定量分析。
