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测定职业接触有机磷农药的人群及普通人群尿中烷基磷酸酯的分析方法。

Analytical method for the determination of urinary alkylphosphates in subjects occupationally exposed to organophosphorus pesticides and in the general population.

作者信息

Aprea C, Sciarra G, Lunghini L

机构信息

Institute of Occupational Medicine, University of Siena, Italy.

出版信息

J Anal Toxicol. 1996 Nov-Dec;20(7):559-63. doi: 10.1093/jat/20.7.559.

Abstract

The determination of urinary alkylphosphates monitors occupational exposure to organophosphorus pesticides and insecticides. This paper describes a method for the quantitative determination of the following metabolites: O,O-dimethylphosphate (DMP), O,O-diethylphosphate (DEP), O,O-diethyldithiophosphate (DETP), O,O-dimethyldithiophosphate (DMDTP), O,O-diethyldithiophosphate (DEDTP), and O,O-dimethylthiophosphate (DMTP). The compounds are derivatized with pentafluorobenzylbromide into pentafluorobenzyl esters which are determined by gas chromatography with a capillary column of intermediate polarity and a flame photometric detector specific for phosphorus. Before the analytical gas chromatographic stage, the urinary extracts are purified on isolute SPE CN columns. The proposed method has a limit of detection of 2-3 micrograms/L at 62.5 micrograms/L and a mean recovery of the purification stage of 85.8-101.0% for all six compounds. The coefficient of variation of the analytical procedure was 7.9-11.9% for the six compounds. The low detection limits make this method suitable also for determining the six metabolites in the general population.

摘要

尿中烷基磷酸酯的测定可监测职业性接触有机磷农药和杀虫剂的情况。本文描述了一种定量测定以下代谢物的方法:O,O-二甲基磷酸酯(DMP)、O,O-二乙基磷酸酯(DEP)、O,O-二乙基二硫代磷酸酯(DETP)、O,O-二甲基二硫代磷酸酯(DMDTP)、O,O-二乙基二硫代磷酸酯(DEDTP)和O,O-二甲基硫代磷酸酯(DMTP)。这些化合物用五氟苄基溴衍生化为五氟苄基酯,通过具有中等极性的毛细管柱和对磷具有特异性的火焰光度检测器的气相色谱法进行测定。在进行分析气相色谱阶段之前,尿提取物在isolute SPE CN柱上进行纯化。所提出的方法在62.5微克/升时的检测限为2 - 3微克/升,所有六种化合物在纯化阶段的平均回收率为85.8 - 101.0%。六种化合物分析过程的变异系数为7.9 - 11.9%。低检测限使得该方法也适用于测定普通人群中的这六种代谢物。

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