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基质固相分散萃取-气相色谱法同时检测人参中五氯硝基苯及其代谢物残留
引用本文:李晶,董丰收,刘新刚,姚建仁,郑永权.基质固相分散萃取-气相色谱法同时检测人参中五氯硝基苯及其代谢物残留[J].农业环境保护,2009(1):216-220.
作者姓名:李晶  董丰收  刘新刚  姚建仁  郑永权
作者单位:中国农业科学院植物保护研究所农业部农药化学与应用技术重点开放实验室,北京100094
摘    要:采用基质固相分散萃取-气相色谱(MsPD—Gc)技术,建立了人参中五氯硝基苯(PcNB)及其代谢物五氯苯胺(PcA)和甲基五氯苯基硫醚(PcTA)残留的多残留分析方法。将人参样品与弗罗里硅土(m/m,1:2)充分研磨5min后装入10mL玻璃注射器内,通过正己烷:丙酮(V/V,5:5)混合溶液洗脱实现了人参中五氯硝基苯及其代谢物的同时提取和净化。结果表明,应用该方法测定人参中五氯硝基苯、五氯苯胺及甲基五氯苯基硫醚,回收率为89.41%~104.42%,相对标准偏差为3.73%-7.43%,五氯硝基苯及其代谢物的方法检出限均小于2ug·kg^-1。

关 键 词:基质固相分散-气相色谱法  人参  残留  五氯硝基苯  代谢物

Simultaneous Determination of Pentachloronitrobenzene Residue and Its Metabolites Pentachloroaniline and Pentachlorothioanisole in Ginseng Based on Matrix Solid Phase Dispersion and Gas Chromatography
LI Jing,DONG Feng-shou,LIU Xin-gang,YAO Jian-ren,ZHENG Yong-quan.Simultaneous Determination of Pentachloronitrobenzene Residue and Its Metabolites Pentachloroaniline and Pentachlorothioanisole in Ginseng Based on Matrix Solid Phase Dispersion and Gas Chromatography[J].Agro-Environmental Protection,2009(1):216-220.
Authors:LI Jing  DONG Feng-shou  LIU Xin-gang  YAO Jian-ren  ZHENG Yong-quan
Institution:(Institute of Plant Protection, Chinese Academy of Agricultural Science, Key Laboratory of Pesticied Chemistry & Application Technology, Ministry of Agriculture, Beijing 100094, China)
Abstract:An effective and simple method for simultaneous determination of pentachloronitrobenzene (PCNB)residue and its metabolites pentachloroaniline (PCA), pentachlorothioanisole (PCTA) in ginseng was developed based on matrix solid-phase dispersion and gas chromatography. Dry ground ginseng samples and florisil sorbent( 1:2 )were homogenized in a mortar for 5 rain and then packed into a 10 mL of glass syringe. Eluted with hexane/acetone=5:5 (V/V)solution, pentachloronitrobenzene and its metabolites were simultaneously extracted and cleaned up. The qualitative and the quantitative analysis of samples was accomplished using gas chromatography with ECD(electronic cap- ture detector). The average recovery and relative standard deviation of PCNB, PCA and PCTA in ginseng at the spiked levels of 0.01, 0.05 and 0.1 mg·kg^-1 was within 89.41%-104.42% and 3.73%-7.43% respectively. The limits of detection(LOD) of the method were 1.88, 1.50, 1.25ug·kg^-1 for PCNB, PCA and PCTA respectively. The proposed method was successfully applied to the determination of PCNB and its metabolites PCA and PCTA in ginseng with satisfactory results.
Keywords:MSPD-GC  ginseng  residues  pentachloronitrobenzene  metabolites
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