Analytical Sciences

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

Takeshi SAITO,*1 Hiromichi AOKI,*1 Akira NAMERA,*2 Hiroshi OIKAWA,*3 Shota MIYAZAKI,*3 Akihiro NAKAMOTO,*4 and Sadaki INOKUCHI*1

*1 Department of Emergency and Critical Care Medicine, Tokai University School of Medicine, 143 Shimokasuya, Isehara, Kanagawa 259-1143, Japan
*2 Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University, 1-2-3 Kasumi, Minami, Hiroshima 734-8551, Japan
*3 GL Sciences Inc., 237-2 Sayamagahara, Iruma, Saitama 358-0032, Japan
*4 Forensic Science Laboratory, Hiroshima Prefectural Police Headquarters, 2-26-3 Kohnan, Naka, Hiroshima 730-0825, Japan

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.

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