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We have developed a rapid, sensitive, and reliable method for simultaneous determination of the urinary metabolites of common insecticides in a single analytical run using gas chromatography–mass spectrometry (GCMS). Thirteen metabolites, one originating from carbamate, six from organophosphates, and seven from pyrethroids, were selected for method validation. Samples at different concentrations (0.5–15 μg/L) were prepared by mixing working solutions containing the analytes with blank urine. After acid hydrolysis for 45 min at 90 ◦C, samples were processed with liquid–liquid extraction and derivatization by N-tert-butyldimethylsilyl-N-methyltrifluoroacetamide (MTBSTFA) before analysis on GCMS. The limits of detection for all thirteen analytes were below 0.1 μg/L. The recovery rates, evaluated at two concentrations (1, 10 μg/L), were found to be 90.48%, on average. The precision of multiple analyses at three different concentrations (0.5, 5, 15 μg/L) within one day or between 10 days was evaluated, and the resultant relative standard deviations were 8.1% or under. We also applied this method to analyze genuine urine samples collected from 30 human subjects, and successfully detected all the metabolites, with detection frequencies more than 50% for pyrethroid metabolites. In summary, this method is not only as good as others in performance, but is advantageous in terms of cost effectiveness and multiplicity of analytes.

Simultaneous Determination of Pyrethroid, Organophosphate and Carbamate Metabolites in Human Urine by Gas Chromatography–Mass Spectrometry (GCMS)