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目的建立地表水中23种有机氯农药(OCPs)的全自动固相萃取-气相色谱-高分辨质谱(GC-HRMS)联用测定方法。方法水样经HLB固相萃取柱富集提取(流速选择10 ml/min),乙酸乙酯和二氯甲烷联合洗脱,氮吹浓缩后,采用GC-HRMS法进样分析。结果 23种有机氯农药在0.152~20.0 ng/L的范围内,所得回归方程均呈良好的线性关系(r≥0.997)。方法的检出限为0.031~0.152 ng/L,定量下限为0.110~0.511 ng/L,平均回收率为70.4%~121.0%,RSD为2.3%~19.4%。结论该方法操作简单,灵敏度高,选择性强,适用于同时测定地表水中23种有机氯农药。
Objective To establish a method for the simultaneous determination of 23 organochlorine pesticides (OCPs) in surface water by gas chromatography-mass spectrometry (GC-HRMS). Methods The aqueous samples were collected by HLB SPE (flow rate 10 ml / min), combined with ethyl acetate and dichloromethane, and concentrated by nitrogen. The samples were analyzed by GC-HRMS. Results The results showed that the regression equation of 23 organochlorine pesticides showed a good linear relationship (r ≥ 0.997) within the range of 0.152-20.0 ng / L. The detection limits were 0.031 ~ 0.152 ng / L, the limits of quantification was 0.110 ~ 0.511 ng / L, the average recoveries were 70.4% ~ 121.0% and the RSDs were 2.3% ~ 19.4%. Conclusion The method is simple, sensitive and selective. It is suitable for simultaneous determination of 23 organochlorine pesticides in surface water.