色谱

色谱 ›› 2012, Vol. 30 ›› Issue (01): 14-20.DOI: 10.3724/SP.J.1123.2011.09019

• 研究论文 • 上一篇    下一篇

气相色谱-串联质谱法测定人参和黄芪中7种毒杀芬残留量

田绍琼1,2, 毛秀红2, 苗水2, 郏征伟2, 王柯2, 季申2*   

  1. 1. 上海医药工业研究院, 上海 200040; 2. 上海市食品药品检验所, 上海 201203
  • 收稿日期:2011-09-16 修回日期:2011-10-24 出版日期:2012-01-28 发布日期:2012-03-01
  • 通讯作者: 季申,主任药师. Tel: (021)50798195,

Determination of seven toxaphene congeners in Ginseng and Milkvetch Root by gas chromatography-tandem mass spectrometry

TIAN Shaoqiong1,2, MAO Xiuhong2, MIAO Shui2, JIA Zhengwei2, WANG Ke2, JI Shen2*   

  1. 1. Shanghai Institute of Pharmaceutical Industry, Shanghai 200040, China; 2. Shanghai Institute for Food and Drug Control, Shanghai 201203, China
  • Received:2011-09-16 Revised:2011-10-24 Online:2012-01-28 Published:2012-03-01

PDF

411

被引次数

49

摘要： 建立了人参和黄芪中毒杀芬代表性单体残留量的检测方法。选择7种指示性毒杀芬单体为检测品种,样品用环己烷-丙酮(9:1,v/v)加速溶剂萃取法提取,经弗罗里硅土固相萃取柱净化后,以气相色谱-电子轰击离子源串联质谱(GC-EI-MS/MS)在多反应监测(MRM)模式下进行测定。在人参和黄芪两种中药材样品基质,0.005、0.01和0.1 mg/kg 3个加标水平条件下,7种毒杀芬单体的回收率为72.4%～105%,相对标准偏差为0.96%～10.4%;方法的检出限(S/N=3)为0.2～1.7 μg/kg,均符合农药残留检测要求。该方法提取效果好,检测灵敏度高,适用于人参和黄芪中7种毒杀芬残留量的检测。

关键词: 残留, 毒杀芬, 黄芪, 气相色谱-电子轰击离子源串联质谱法, 人参, 中药材

Abstract: A novel method for the determination of representative toxaphene congeners in traditional Chinese herbal medicines was developed. Ginseng and Milkvetch Root were selected as the samples and seven toxaphene congeners were selected as the monitoring objects. The samples were extracted by accelerated solvent extraction with cyclohexane-acetone (9:1, v/v), then cleaned-up by Florisil solid phase extraction with hexane as the eluent and the residues were detected by gas chromatography-electron ionization tandem mass spectrometry (GC-EI-MS/MS) in multiple reaction monitoring (MRM) mode. The performance was demonstrated by the analysis of Ginseng and Milkvetch Root samples spiked with toxaphene congeners at three concentration levels of 0.005, 0.01 and 0.1 mg/kg. The recoveries ranged from 72.4% to 105% with the relative standard deviations (RSDs) of 0.96%~10.4%. The limits of detection (LODs) were 0.2~1.7 μg/kg. This method is sensitive and efficient in the aspect of extraction, and can be applied to monitor the residue of toxaphene congeners in Ginseng and Milkvetch Root.

Key words: Ginseng, Milkvetch Root, residue, toxaphene, traditional Chinese herbal medicine, gas chromatography-electron ionization tandem mass spectrometry(GC-EI-MS/MS)