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微波辅助萃取结合分散固相萃取和气相色谱法同时测定中药材中的有机磷农药

Simultaneous determination of organophosphorus pesticides in Chinese herbal medicines by microwave-assisted extraction coupled with dispersive-solid phase extraction and gas chromatography.

作者信息

Wan Yi-Qun, Mao Xue-Jin, Yan Ai-Ping, Shen Ming-Yue, Wu Yu-Mei

机构信息

Nanchang University, China.

出版信息

Biomed Chromatogr. 2010 Sep;24(9):961-8. doi: 10.1002/bmc.1393.

Abstract

A reliable, rapid and nontoxic analytical method was proposed for the simultaneous determination of 16 organophosphorus pesticides in Chinese herbal medicines. The pesticides were extracted by ethanol and the experimental variables, such as temperature, extraction time and volume of ethanol, were optimized through orthogonal array experimental design. Cleanup of extracts was performed with dispersive-solid phase extraction using primary secondary amine as the sorbent. The determination of pesticides in the final extracts was carried out by gas chromatography-flame photometric detection. Under optimized conditions the obtained recoveries, except for isocarbophos, were in the range 73.8-123%, with relative standard deviations equal to or lower than 15.2% and limits of detection ranging from 0.001 to 0.009 mg/kg.

摘要

提出了一种可靠、快速且无毒的分析方法,用于同时测定中药材中的16种有机磷农药。采用乙醇提取农药,并通过正交试验设计对温度、提取时间和乙醇体积等实验变量进行了优化。以伯仲胺为吸附剂,采用分散固相萃取法对提取物进行净化。最终提取物中的农药通过气相色谱-火焰光度检测法进行测定。在优化条件下,除水胺硫磷外,回收率在73.8%-123%之间,相对标准偏差等于或低于15.2%,检测限在0.001至0.009 mg/kg之间。

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