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目的建立采用分散固相萃取和在线凝胶渗透色谱-气相色谱-质谱法(GPC-GC-MS)测定香港中成药中20种有机氯农药残留的分析方法。方法样品经乙腈涡旋提取,加入N-丙基乙二胺(primary-secondary amine,PSA)、C18-N进行分散固相萃取净化后,经在线凝胶渗透色谱(gel permeation chromatography,GPC)净化,采用气相色谱与质谱串联技术在离子检测方式下测定,以保留时间和特征离子进行目标成分的定性鉴别,以外标法定量。结果 20种有机氯农药在质量浓度2~100μg·L-1内均呈良好的线性关系,相关系数为0.999 1~0.999 9;3个水平加标回收率为83.8%~112.9%,RSD(n=3)为1.4%~8.1%;检出限为0.04×10-9%~0.76×10-9%,定量限为0.13×10-9%~2.52×10-9%,进样精密度为1.2%~3.0%。结论本方法的灵敏度、准确度和精密度均符合农药多残留检测技术要求,适用于香港中成药中20种有机氯农药残留的检测。
Objective To establish a method for the determination of 20 organochlorine pesticide residues in Chinese proprietary medicines in Hong Kong by dispersive solid-phase extraction and on-line gel permeation chromatography-gas chromatography-mass spectrometry (GPC-GC-MS). Methods The samples were extracted with acetonitrile by vortex and purified by dispersive solid-phase extraction after adding primary-secondary amine (PSA) and C18-N, and purified by gel permeation chromatography (GPC) , Using gas chromatography and tandem mass spectrometry in ion detection mode to determine the retention time and characteristic ions of the target component of the qualitative identification, external standard method. Results The 20 organochlorine pesticides showed a good linearity in the range of 2 ~ 100 μg · L-1 with the correlation coefficient of 0.999 1 ~ 0.999 9. The recoveries of three organochlorine pesticides ranged from 83.8% to 112.9% with RSD (n = 3) was 1.4% ~ 8.1%. The detection limits were 0.04 × 10-9% ~ 0.76 × 10-9%. The limits of quantification were 0.13 × 10-9% ~ 2.52 × 10-9% 1.2% ~ 3.0%. Conclusion The sensitivity, accuracy and precision of this method are in line with the requirements of pesticide multi-residue detection technology and suitable for the detection of 20 organochlorine pesticide residues in Chinese proprietary medicines in Hong Kong.