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0.2～1.7μg/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。
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 sam- pies 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.
出处
《色谱》
CAS
CSCD
北大核心
2012年第1期14-20,共7页
Chinese Journal of Chromatography
关键词
气相色谱-电子轰击离子源串联质谱法
毒杀芬
残留
人参
黄芪
中药材
gas chromatography-electron ionization tandem mass spectrometry（GC-EI-MS/MS）
toxaphene
residue
Ginseng
Milkvetch Root
traditional Chinese herbal medicine
