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气相色谱法测定人血浆、小鼠血浆、组织及脂肪中的谷硫磷乙酯。

Gas-liquid chromatographic determination of azinphos ethyl in human plasma and in mouse plasma, tissue, and fat.

作者信息

Stein V B, Pittman K A

出版信息

J Assoc Off Anal Chem. 1976 Sep;59(5):1094-6.

PMID:965333
Abstract

A new method for the determination of azinphos ethyl (O,O-diethyl-S-(4-oxo-1,2,3-benzotriazin-3(4H)-ylmethyl) phosphorodithioate) in human plasma and in mouse plasma, tissue, and fat has been developed. The method is based on extraction with benzene or hexane and cleanup of fat and tissue samples by a minicolumn containing Florisil and sodium sulfate. Azinphos ethyl is eluted from the column with 10% acetonitrile in benzene and is concentrated to an appropriate volume for gas-liquid chromatographic analysis, using a 63Ni electron capture detector and a glass column containing 3% OV-1 on Gas-Chrom Q. The method is sensitive to 0.005 ppm in human plasma, 0.01 ppm in mouse plasma, 0.08 ppm in mouse liver, 0.05 ppm in mouse brain, and 0.10 ppm in mouse fat. The limit of detection is 2 pg; mean recoveries ranged from 96 to 98%.

摘要

已开发出一种测定人血浆以及小鼠血浆、组织和脂肪中谷硫磷乙酯(O,O - 二乙基 - S - (4 - 氧代 - 1,2,3 - 苯并三嗪 - 3(4H)-基甲基) 二硫代磷酸酯)的新方法。该方法基于用苯或己烷萃取,并通过装有弗罗里硅土和硫酸钠的微柱对脂肪和组织样品进行净化处理。谷硫磷乙酯用含10%乙腈的苯从柱中洗脱出来,并浓缩至合适体积用于气液色谱分析,使用63Ni电子捕获检测器和装有3% OV - 1(涂覆在Gas - Chrom Q上)的玻璃柱。该方法对人血浆中谷硫磷乙酯的检测灵敏度为0.005 ppm,小鼠血浆中为0.01 ppm,小鼠肝脏中为0.08 ppm,小鼠脑中为0.05 ppm,小鼠脂肪中为0.10 ppm。检测限为2 pg;平均回收率在96%至98%之间。

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