QuEChERS-凝胶渗透色谱/气相色谱-质谱法同时测定降尘中18种有机氯农药

Determination of Eighteen Organochlorine Pesticides in Dust by QuEChERS-GPC/GC-MS

建立了在线凝胶渗透色谱/气相色谱-质谱（GPC/GC-MS）测定大气降尘中18种有机氯农药残留的分析方法。样品经过简化QuEChERS方法处理后，经乙腈萃取，石墨化炭黑（GCB）净化，一步离心后过膜上机检测。采用该方法能在30 min内处理8-10个样品，配合GPC净化，不仅缩短了分析时间，而且提高了工作效率和结果的准确性。检测结果表明,18种有机氯农药在0.025-2.0 mg/L质量浓度范围内线性关系良好，相关系数为0.991 9-0.999 6，样品检出限为3.2-14.6 μg/kg，定量下限为10.7-48.7 μg/kg。在0.2、1.0 mg/kg 2个加标水平下，18种有机氯农药的平均回收率为78.6%-117.3%，相对标准偏差（RSD，n=5）为1.3%-5.1%。

An on-line gel permeation chromatography combined with gas chromatography-mass spectrometric（GPC/GC-MS） method was developed for the determination of eighteen organochlorine pesticides in atmospheric dust.The sample was simplified by QuEChERS method,extracted with acetonitrile and cleaned with graphitized carbon black（GCB）,then filtrated by one step of centrifugation before detection.By this method,8-10 samples can be treated within 30 min,and after coupled with GPC purification,the analysis time could be shortened,and the working efficiency and the accuracy of results could be improved.The result indicated that the calibration curves were liner in the range of 0.025-2.0 mg/L, with correlation coefficients of 0.991 9-0.999 6.The limits of detection for the sample were in the range of 3.2-14.6 μg/kg and the limits of quantitation were 10.7-48.7 μg/kg.The mean recoveries of eighteen organochlorine pesticides at spiked levels of 0.2,1.0 mg/kg were in the range of 78.6%-117.3%,with relative standard deviations（RSDs,n=5） of 1.3%-5.1%.