地表水中23种有机氯农药的自动固相萃取-气相色谱-高分辨质谱联用测定法

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。

Determination of 23 organochlorine pesticides in surface water by automatic solid phase extraction-gas chromatography-high resolution mass spectrometry

Objective To establish a sensitive and accurate method for the simultaneous determination of 23 organochlorine pesticides (OCPs) in surface water by automatic solid phase extraction-gas chromatography-high resolution mass spectrometry (GC-HRMS).Methods The water samples were concentrated by HLB columns (the flow rate was 10 ml/min) and extracted with the mixture of dichloromethane and aceticether.The final eluate was concentrated and detected with gas chromatographyhigh resolution mass spectrometry(GC-HRMS).Results The calibration curves of 23 organochlorine pesticides showed a good linearity in the range of 0.152-20.0 ng/L,the correlation coefficients were uore than 0.997.The limits of detection (LOD) of OCPs were 0.031-0.152 ng/L,the limits of quantification (LOQ) of OCPs were 0.1 10-0.511 ng/L.The spiked recoveries ranged from 70.4％ to 121.0％,and the relative standard deviations ranged from 2.3％ to 19.4％.Conclusion The method is easy,accurate,sensitive and applicable to the simultaneous determination of 23 mganochlorine pesticides(OCPs) in surface water.