分散固相萃取-气相色谱法测定山茱萸中20种农药残留Determination of twenty pesticide residues in Cornus officinals by gas chromatography using dispersive solid phase extraction
张舒婷,陈晓辉,于治国,沈旭,勾萌,毕开顺
ZHANG Shu-ting,CHEN Xiao-hui,YU Zhi-guo,SHEN Xu,GOU Meng,BI Kai-shun(School of Pharmacy
摘要(Abstract):
目的建立分散固相萃取气相色谱法测定山茱萸中有机氯和拟除虫菊酯类农药残留的方法。方法选用乙腈为提取溶剂,丙基乙二胺(PSA)为分散净化剂;采用Hp-5毛细管气相色谱柱分离,电子捕获检测器进行检测。结果有机氯和拟除虫菊酯分别在5~500μg.L-1和10~1 000μg.L-1内呈良好线性关系,相关系数均大于0.997 8;检定量限为1~5μg.L-1;平均回收率为78.32%~112.80%,RSD为3.2%~9.4%。结论本方法适用于中药材中的农药多残留的测定与安全监控。
Objective To establish a gas chromatography method for simultaneous determination of organochlorine and pyrethroid pesticide residues in Cornus officinals by dispersive solid phase extraction(DSPE).Methods Pesticides were extracted with acetonitrile and the primary secondary amine(PSA)was chosen as the adsorbent.The gas chromatography was used with electron capture detector and the separation was performed on an Hp-5 column.The pesticide residues were calculated by external standard method.Results Good linear relation was obtained over the range of 5-500 μg·L-1 for organochlorine and 10-1 000 μg·L-1 for pyrethroid.The limit of detection was 1-5 μg·L-1.The average recoveries of organochlorine and pyrethroid were 78.32%-112.80% with corresponding RSD of 3.2%-9.4%.Conclusions The sample and rapid method is applied to pesticide residues detection and security monitoring and control.
关键词(KeyWords):
分散固相萃取法;丙基乙二胺;气相色谱法;有机氯;拟除虫菊酯;山茱萸
dispersive solid phase extraction;primary secondary amine;gas chromatography;organochlorine;pyrethroid;Cornus officinals
基金项目(Foundation):
作者(Author):
张舒婷,陈晓辉,于治国,沈旭,勾萌,毕开顺
ZHANG Shu-ting,CHEN Xiao-hui,YU Zhi-guo,SHEN Xu,GOU Meng,BI Kai-shun(School of Pharmacy
DOI: 10.14066/j.cnki.cn21-1349/r.2010.03.001
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- 分散固相萃取法
- 丙基乙二胺
- 气相色谱法
- 有机氯
- 拟除虫菊酯
- 山茱萸
dispersive solid phase extraction - primary secondary amine
- gas chromatography
- organochlorine
- pyrethroid
- Cornus officinals