Analytical Method for the Determination of Urinary Alkylphosphates in Subjects Occupationally Exposed to Organophosphorus Pesticides and in the General Population

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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-diethylthiophosphate (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 µg/L at 62.5 µg/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.

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