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采用凝胶渗透色谱法和弗罗里硅土柱净化相结合,以及气相色谱/质谱联用技术同时测定糙米中的109种农药。

Simultaneous determination of 109 pesticides in unpolished rice by a combination of gel permeation chromatography and Florisil column purification, and gas chromatography/mass spectrometry.

作者信息

Zhang Wei-Guo, Chu Xiao-Gang, Cai Hui-Xia, An Juan, Li Chong-Jiu

机构信息

College of Science, China Agricultural University, Beijing 100094, PR China.

出版信息

Rapid Commun Mass Spectrom. 2006;20(4):609-17. doi: 10.1002/rcm.2341.

Abstract

A multi-residue method is described for the simultaneous analysis of 109 pesticides with different properties in unpolished rice. The range covers organophosphorus, organochlorine, carbamate, and synthetic pyrethroid pesticides. The pesticides were extracted from the sample using ethyl acetate. Most higher molecular weight components such as lipids in the co-extractives were removed by gel permeation chromatography (GPC) with a Bio-bead SX-3 column. A Florisil column with ethyl acetate/hexane as the eluting solvents was used for further cleanup. The pesticides were finally simultaneously determined by gas chromatography/mass spectrometry (GC/MS) in selective ion monitoring (SIM) mode. The average recoveries for most pesticides (spiked level 0.02, 0.1 and 1 microg/g) ranged from 70% to 110%, the relative standard deviation (RSD) was below 20% in every case, and the limit of detection (LOD) varied from 1 to 20 ng/g.

摘要

描述了一种用于同时分析糙米中109种具有不同性质农药的多残留方法。该范围涵盖有机磷、有机氯、氨基甲酸酯和拟除虫菊酯类农药。使用乙酸乙酯从样品中提取农药。共提取物中大多数较高分子量的成分,如脂质,通过使用Bio-bead SX-3柱的凝胶渗透色谱法(GPC)去除。以乙酸乙酯/己烷为洗脱溶剂的弗罗里硅土柱用于进一步净化。最终通过气相色谱/质谱联用仪(GC/MS)在选择性离子监测(SIM)模式下同时测定农药。大多数农药(加标水平为0.02、0.1和1微克/克)的平均回收率在70%至110%之间,每种情况下相对标准偏差(RSD)均低于20%,检测限(LOD)在1至20纳克/克之间变化。

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