title: 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.
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-C(18) 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.
authors: Department of Emergency and Critical Care Medicine, Tokai University School of Medicine, Isehara, Kanagawa, Japan. saito@is.icc.u-tokai.ac.jp
authors: Takeshi
authors: T
authors: Saito
authors: Hiromichi
authors: H
authors: Aoki
authors: Akira
authors: A
authors: Namera
authors: Hiroshi
authors: H
authors: Oikawa
authors: Shota
authors: S
authors: Miyazaki
authors: Akihiro
authors: A
authors: Nakamoto
authors: Sadaki
authors: S
authors: Inokuchi
mesh_terms: D000613:Aminobutyrates / Q000097:blood* / Q000652:urine*; D008401:Gas Chromatography-Mass Spectrometry; D005998:Glycine / Q000031:analogs & derivatives* / Q000097:blood / Q000652:urine; D006801:Humans; D009943:Organophosphorus Compounds / Q000097:blood* / Q000652:urine*; D011109:Polymethacrylic Acids / Q000737:chemistry; D012680:Sensitivity and Specificity; D014025:Titanium / Q000737:chemistry; D000097797:Glyphosate
chemical_list: D000613:Aminobutyrates; D005998:Glycine; D009943:Organophosphorus Compounds; D011109:Polymethacrylic Acids; D014025:Titanium; D000097797:Glyphosate; C009495:titanium dioxide; C003121:phosphinothricin