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采用自动化凝胶渗透色谱净化/气相色谱-质谱法分析花生中的农药多残留。

Pesticide multiresidue analysis of peanuts using automated gel permeation chromatography clean-up/gas chromatography-mass spectrometry.

机构信息

Ocean University of China, Shandong, China.

出版信息

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2009 Mar;26(3):333-9. doi: 10.1080/02652030802350672.

Abstract

A method based on automated gel permeation chromatography (GPC) and on-line quantitative concentration was developed for the determination of residues of 38 typically used pesticides in high-oil peanuts. Pesticides were extracted using acetonitrile into an oil fraction containing little of the peanut matrix. After changing the solvent to the mobile phase (1 : 1 cyclohexane : ethyl acetate), clean-up was carried out using GPC, the final collected solution being automatically concentrated to a fixed volume and transferred into vials for gas chromatography (GC) injection. The pesticides were analysed by gas chromatography-mass spectrometry (GC/MS) in the selected ion monitoring (SIM) mode. Average recoveries (spiked levels of 0.02, 0.05, and 0.1 microg g(-1)) were between 70 and 117%. The relative standard deviation of the method was 3.5-21% (n = 6). This approach gave comparable results with a previously published method.

摘要

建立了一种基于自动化凝胶渗透色谱(GPC)和在线定量浓缩的方法,用于测定高脂肪花生中 38 种常用农药的残留量。使用乙腈将农药提取到含有少量花生基质的油相中。在将溶剂改为流动相(1:1 环己烷:乙酸乙酯)后,使用 GPC 进行净化,最后收集的溶液自动浓缩至固定体积,并转移到小瓶中进行气相色谱(GC)进样。采用气相色谱-质谱(GC/MS)在选择离子监测(SIM)模式下分析农药。平均回收率(添加水平为 0.02、0.05 和 0.1μg g(-1))在 70%至 117%之间。该方法的相对标准偏差为 3.5-21%(n=6)。与先前发表的方法相比,该方法具有相当的结果。

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