广西科学2019，Vol.26Issue(5)：532-538,7.DOI:10.13656/j.cnki.gxkx.20191024.002
GC-ECD法测定中药配方颗粒中20种有机氯农药残留量
Determination of 20 Kinds of Organochlorine Pesticide Residues in Chinese Dispensing Granules by GC-ECD
摘要
Abstract
To establish a GC-ECD method to determine 20 kinds of organochlorine pesticide residues[benzene hexachloride (α-BHC,β-BHC,γ-BHC,δ-BHC)DDT(pp'-DDE,pp'-DDD,pp'-DDT,op'-DDT) PCNB，aldrin，heptachlor，heptachlor epoxide，endrin，dieldrin，hexachlorobenzene，pentachlorophe-nol aniline，methylpentachlorophenyl sulfide，cis-chlordane，trans-chlordane，oxy-chlordane] in Chinese dispensing granules. Chinese dispensing granules samples were ultrasonically extracted with ethyl acetate，and the extract was purified through Florisil solid phase extraction(SPF) cartridge，and then treated with sulfuric acid to remove the impurities. GC was performed on DB-5 gas capillary column(the column length 60 m，inner diameter 0. 25mm，thickness of film 0. 25μm)with electron capture detector. The methods used were temperature programming and ECD detector detection. The internal standard method was used for quantitative analysis. The inlet temperature was 250℃ and the detector temperature was 300℃.The carrier gas was high purity nitrogen at a flow rate of 1.0 mL·min-1.The pulse was not split injection，and the injection volume was 1 μL. The results showed that there were good linear relationships between 20 pesticide components at 2~100 μg/L. The spiked recovery rates of 20 pesticides were in the range of 71 .37% to 118.06%，and the relative standard deviation(RSD) was 1.19% to 7. 88%.The method is simple and accurate，and can be applied to the simultaneous detection of 20 organochlorine pesticide residues in Chinese dispensing granules.关键词
中药配方颗粒/有机氯农药/GC-ECD/Florisil固相萃取/硫酸Key words
Chinese dispensing granules/organochlorine pesticide residues/GC-ECD/Florisil solid phase extraction/sulfuric acid分类
医药卫生引用本文复制引用
白桂昌,吕轶峰,罗轶,何颂华..GC-ECD法测定中药配方颗粒中20种有机氯农药残留量[J].广西科学,2019,26(5):532-538,7.基金项目
广西特聘专家专项经费项目和广西壮瑶民族药中外源性有害残留物检测技术研究平台(广西壮族自治区食品药品监督管理局 2016 年直属单科研项目补充立项项目,桂食药监科评函〔2016〕44 号)资助. （广西壮族自治区食品药品监督管理局 2016 年直属单科研项目补充立项项目,桂食药监科评函〔2016〕44 号）
