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气相色谱-质谱联用技术在人参中有机氯农药残留量测定中的应用

[Application of gas chromatography-mass spectrometry for determination of the organochlorine pesticide residues in ginseng].

作者信息

Zhao Y, Chen J, Wang X

机构信息

Institute of Nutrition and Food Hygiene, Chinese Academy of Preventive Medicine, Beijing 100050, China.

出版信息

Wei Sheng Yan Jiu. 1999 Jan 30;28(1):53-4.

PMID:12712751
Abstract

A gas chromatographic-electronionization-mass spectrometric method (GC-EIMS) was developed for the determination of organochlorine pesticide residues in Ginseng plants. The Ginseng samples were extracted with acetone, partioned using petroleum ester with sodium chloride saturated aqueous solution and clean-up with concentrated sulfuric acid. The organochlorine pesticide residues were analysed by GC-MS with monitoring selective mass ions. Ten organochlorine pesticides including alpha, beta, gamma and delta isomers of hexachlorocyclohexane (HCH), pp'-DDE, pp'-DDT, op'-DDT, pp'-DDT, pentachloronitrobenzene (Quintozene, PCNB), and hexachlorobenzene(HCB), were determined simultaneously. Targeted pesticide analytes were separated on DB-5 capillary column. The optimum chromatographic conditions and MS parameters were determined. The average recovery rates for those pesticide residues Ginseng were from 76.6% to 90.1% at 0.1 mg/kg of spiked level, except 58.3% for PCNB. The relative standard deviations were 9.3%-15.0%.

摘要

建立了一种气相色谱 - 电子电离 - 质谱法(GC - EIMS)用于测定人参植株中有机氯农药残留量。人参样品用丙酮提取,用石油醚与氯化钠饱和水溶液进行分配,并用浓硫酸净化。通过气相色谱 - 质谱联用仪监测选择性质量离子来分析有机氯农药残留量。同时测定了包括六氯环己烷(HCH)的α、β、γ和δ异构体、pp'-DDE、pp'-DDT、op'-DDT、pp'-DDT、五氯硝基苯( quintozene,PCNB)和六氯苯(HCB)在内的10种有机氯农药。目标农药分析物在DB - 5毛细管柱上分离。确定了最佳色谱条件和质谱参数。在0.1 mg/kg的加标水平下,人参中这些农药残留的平均回收率为76.6%至90.1%,PCNB除外,其回收率为58.3%。相对标准偏差为9.3% - 15.0%。

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