Mix-mode TiO-C18 Monolith Spin Column Extraction and GC-MS for the Simultaneous Assay of Organophosphorus Compounds and Glufosinate, and Glyphosate in Human Serum and Urine

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  • SAITO Takeshi
    Department of Emergency and Critical Care Medicine, Tokai University School of Medicine
  • AOKI Hiromichi
    Department of Emergency and Critical Care Medicine, Tokai University School of Medicine
  • NAMERA Akira
    Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University
  • OIKAWA Hiroshi
    GL Sciences Inc.
  • MIYAZAKI Shota
    GL Sciences Inc.
  • NAKAMOTO Akihiro
    Forensic Science Laboratory, Hiroshima Prefectural Police Headquarters
  • INOKUCHI Sadaki
    Department of Emergency and Critical Care Medicine, Tokai University School of Medicine

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Abstract

A rapid, specific, and sensitive method for the simultaneous quantitation of organophosphates (fenitrothion (MEP), malathion, and phenthoate (PAP)), glufosinate (GLUF), and glyphosate (GLYP) in human serum and urine by gas chromatography–mass spectrometry (GC-MS) has been validated. All of the targeted compounds together with the internal standard were extracted from the serum and urine using a mix-mode TiO-C18 monolithic spin column. The recovery of organophosphates from serum and urine ranged from 12.7 to 49.5%. The recovery of GLUF and GLYP from serum and urine ranged from 1.9 to 7.9%. The intra- and inter-accuracy and precision (expressed as relative standard deviation, %RSD) were within 96.7 – 107.7% and 4.0 – 13.8%, respectively. The detection and quantitation limits for serum and urine were 0.1 and 0.1 μg/ml, respectively, for organophosphates, 0.1 and 0.5 μg/ml, respectively for GLUF and GLYP. The method had linear calibration curves ranging from 0.1 to 25.0 μg/ml for organophosphates and 0.5 – 100.0 μg/ml for GLUF, and GLYP. The validated method was successfully applied to a clinical GLYP poisoning case.

Journal

  • Analytical Sciences

    Analytical Sciences 27 (10), 999-, 2011

    The Japan Society for Analytical Chemistry

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