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蛋类中有机氯农药的凝胶渗透与弗罗里硅土柱色谱净化及气相色谱测定

Gel permeation and florisil chromatographic cleanup and gas chromatographic determination of organochlorine pesticides in eggs.

作者信息

Furusawa N, Okazaki K, Iriguchi S, Yamaguchi H, Saitoh M

机构信息

Osaka City University, Faculty of Human Life Science, Japan.

出版信息

J AOAC Int. 1998 Sep-Oct;81(5):1033-6.

PMID:9772745
Abstract

Cleanup of residual organochlorine pesticides (OCPs; alpha-, beta-, gamma-, and delta-BHC; aldrin; dieldrin; p, p'-DDE; o,p'-DDT; p,p'-DDD; and p,p'-DDT) in eggs by gel permeation chromatography (GPC) and Florisil minicolumn chromatography is described. Ten OCPs in purified extract are determined by gas chromatography with electron capture detection. The lipids extracted from whole egg are cleaned up first by GPC with an Envirogel column and an ethyl acetate-cychlohexane (1 + 1, v/v) mobile phase and then by Florisil minicolumn chromatography with 15% (v/v) diethyl ether-hexane eluant. Cleanup is highly efficient. Average recoveries of 10 spiked OCPs (0.0025-0.0125 ppm) ranged from 81 to 101%, with coefficients of variation between 1 and 14%. The detection limit was 0.001 ppm for the 10 OCPs.

摘要

描述了通过凝胶渗透色谱法(GPC)和弗罗里硅土微柱色谱法净化鸡蛋中残留有机氯农药(OCPs;α-、β-、γ-和δ-六六六;艾氏剂;狄氏剂;p,p'-滴滴伊;o,p'-滴滴涕;p,p'-滴滴滴;以及p,p'-滴滴涕)的方法。采用带电子捕获检测的气相色谱法测定纯化提取物中的10种有机氯农药。从全蛋中提取的脂质首先通过装有Envirogel柱和乙酸乙酯 - 环己烷(1 + 1,v/v)流动相的GPC进行净化,然后通过用15%(v/v)乙醚 - 己烷洗脱剂的弗罗里硅土微柱色谱法进行净化。净化效率很高。10种加标有机氯农药(0.0025 - 0.0125 ppm)的平均回收率在81%至101%之间,变异系数在1%至14%之间。这10种有机氯农药的检测限为0.001 ppm。

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