郏征伟 毛秀红 苗 水 陆继伟 陈 钶 王 柯 季 申. 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J. 药学学报, 2010,45(3): 353-358.
引用本文: 郏征伟 毛秀红 苗 水 陆继伟 陈 钶 王 柯 季 申. 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J. 药学学报, 2010,45(3): 353-358.
JIA Zheng-Wei, Mao-Xiu-Gong, Miao- Shui, Liu-Ji-Wei, Chen- Ke, Wang- Ke, Ji- Shen. Simultaneous determination of 56 organochlorine and pyrethroid pesticides in traditional Chinese medicines by GC coupled with dual-tower and dual-columnJ. 药学学报, 2010,45(3): 353-358.
Citation: JIA Zheng-Wei, Mao-Xiu-Gong, Miao- Shui, Liu-Ji-Wei, Chen- Ke, Wang- Ke, Ji- Shen. Simultaneous determination of 56 organochlorine and pyrethroid pesticides in traditional Chinese medicines by GC coupled with dual-tower and dual-columnJ. 药学学报, 2010,45(3): 353-358.

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

  • 摘要:

    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0.01 mg·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。

     

    Abstract:

    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.

     

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