气相色谱双塔双柱法同时测定中药材中56种有机氯类及拟除虫菊酯类农药残留量

Simultaneous determination of 56 organochlorine and pyrethroid pesticides in traditional Chinese medicines by GC coupled with dual-tower and dual-column

研究中药材中有机氯类及拟除虫菊酯类农药残留量的测定方法。样品经高速均质器均质提取,依次经凝胶渗透色谱(GPC)和固相萃取柱(SPE)净化后,用气相色谱双塔双柱进样,双电子捕获检测器同时定性、定量测定。在3种中药材样品基质、3水平添加条件下,56种农药的回收率大多在70.0%～110.0%,相对标准偏差小于15%,检测限大多低于0.01mg·kg-1,符合农药多残留检测的要求。本法净化效果好、基质干扰小、灵敏度高、重现性好,可用于中药材样品中有机氯类及拟除虫菊酯类农药残留量的检测。

The paper is to report the establishment of a method for the determination of multi-residue organochlorine and pyrethroid pesticides in traditional Chinese medicines （TCMs）. Fifty-six pesticides were extracted by high-speed homogenization, and then purified through gel permeation chromatography （GPC） and solid phase extraction （SPE） cartridges. The residues were simultaneously identified and quantified by GC-ECD equipped with dual tower, dual column and two μ-ECD detectors. The analytical performance was demonstrated by the analysis of 3 TCMs samples’ extracts, spiked at three concentration levels for each pesticide. In general, the recoveries ranging from 70% to 110%, with relative standard deviations （RSDs） better than 15%, were obtained. The limit of detection （LOD） for most of the targeted pesticides tested was below 0.01 mg·kg-1. The method had good extraction efficiency, purification effect and good reproducibility, which could be applied to the determination of organochlorine and pyrethroid pesticide residues in the routine analysis of TCMs.