摘要
目的：建立中药材中7种拟除虫菊酯类农药残留的检测方法，为中药材安全使用标准的建立提供科学依据。方法7种农药残留的样品以丙酮超声提取，并采用凝胶渗透色谱（G PC ）和石墨碳柱结合的方法进行净化，选用气相色谱-质谱串联技术（GC/MS）在DB-17MS毛细管柱上用程序升温技术分离和选择离子检测方式，以外标法对样品进行测定。结果7种农药可在13 min内完全分离，在10～1000μg ＆#183; L -1的范围内有良好的线性关系，相关系数在0．9991～0．9999的范围内，检测限为0．9～2．3μg ＆#183; kg -1，3个水平回收率在70％～112％之间，相对标准偏差小于10％（n＝9）。结论该方法灵敏度高，重复性好，适用于中药材中7种农药残留的检测。
Objective To establish an analytical method for the detection of 7 pyrethroid pesticides residue in Chinese herbal medi-cines and supply an evidence for the standard of safety to use traditional Chinese herbs .Methods The sample was extracted with acetone and the extract was cleaned by using GPC and Graphite carbon columns .Based on GC/MS ,the pesticides were separated on a DB-17MS column using a temperature program and were detected with a mass selective detector in selective ion monitoring （SIM） mode .Results 7 pesticides were separated within 13 minutes .Linearities of the 7 kinds pesticides were good（r=0 .999 1-0 .999 9） in ranges of 10-1 000 μg ＆#183; L -1 .The limit of detection was 0 .9-2 .3μg ＆#183; kg -1 .The average spiked recoveries in three lev-els were 70%-112% with relative standard deviation （RSD） less than 10% （n=9） .Conclusion The method is sensitive for the res-idue analysis of 7 pesticides in traditional Chinese herbs .
出处
《西北药学杂志》
CAS
2014年第2期132-134,共3页
Northwest Pharmaceutical Journal
关键词
中药材
农药残留
GPC
GC/MS
Chinese herbal medicines
pesticide residue
GPC
GC/MS
