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

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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。 To study the determination of organochlorine and pyrethroid pesticide residues in Chinese herbal medicines. The samples were homogenized by high-speed homogenizer and purified by gel permeation chromatography (GPC) and solid-phase extraction (SPE) columns. The two-column double-column gas chromatography was used for simultaneous qualitative and quantitative determination of two electron capture detectors . The recoveries of 56 pesticides ranged from 70.0% to 110.0% with relative standard deviations less than 15% and the limits of detection were mostly lower than 0.01 mg · kg-1, which were in line with three pesticides Residue testing requirements. The method has the advantages of good purification effect, small matrix interference, high sensitivity and good reproducibility, and can be used for detecting organochlorine and pyrethroid pesticide residues in samples of Chinese herbal medicines.
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