摘要
目的:建立荭草中12种有机氯和拟除虫菊酯的固相萃取-毛细管气相色谱的分析法。方法:样品以正己烷-丙酮为提取剂,采用超声提取,Florisil固相萃取柱净化。采用HP-5弹性石英毛细管色谱柱(0.32 mm×30 m,0.25μm)程序升温,电子捕获检测器检测,内标法定量。结果:12种农药能在31min内获得良好分离,9种有机氯农药标准品在1～200μg.L-1,3种拟除虫菊酯在5～1 000μg.L-1线性关系良好,相关系数(r)均大于0.996,低、中、高3个添加水平的回收率分别为82.0%～104.4%,79.1%～106.8%,82.1%～106.4%,相对标准偏差(RSD)为0.2%～7.9%,0.8%～6.1%,0.7%～6.1%,检出限为0.15～13μg.kg-1。对15个批次的样品测定结果均未检出有机氯及拟除虫菊酯农药残留。结论:本方法简便快速,适合荭草中痕量的有机氯及拟除虫菊酯农药残留的同时测定。
Objective：The solid phase extraction and capillary gas chromatography were introduced for determining 12 organoehiorinc and pyrethroid pesticide residues in polygonum orientale. Method：The organochlorine and pyrethroid pesticides were extracted with n-hexane and acetone by ultrasonic method and cleaned up by Florisi] solid-phase extraction （SPE） column. Then, the extract was separated by capillary column HP-5 （0.32 mm× 30 m,0.25 μm） and detected by （electron capture detector,ECD）. The internal standards were used for quantitative determination. Result： A mixed standard solution prepared from primary standards of 9 organoehlorine and 3 pyrethroid pesticide. The calibration curve for each of 12 organochlorine and pyrethroid pesticide was prepared covering the concentration ranges of 1 to 200 or 5 to 1 000 μg·L^-1. The average recoveries and RSD were in the range of 82.0% -106.8% and 0.2% -7.9% at three organochlorine and pyrethroid pesticides levels respectively. The limits of detection were 0. 15-13 μg·kg^-1. There were no organochlorine and pyrethroid pesticide detected in 15 batches samples. Conclusion： This method was effective, fast and accurate. It has good repeatability and suitable for the analysis of organochlorine and pyrethroid pesticide in polygonum orientale.
出处
《中国实验方剂学杂志》
CAS
北大核心
2010年第18期47-49,共3页
Chinese Journal of Experimental Traditional Medical Formulae
基金
国家科技重大专项重大新药创制项目(2008ZX09101-021)
国家自然科学基金项目(30860366)
贵州省科技重大专项项目(黔科合重大专项字[2007]6010号)
关键词
荭草
有机氯及拟除虫菊酯
农药残留
polygonum orientale
organochlorine and pyrethroid
pesticide residues
