title: Rapid determination of disulfoton and its oxidative metabolites in human whole blood and urine using QuEChERS extraction and liquid chromatography-tandem mass spectrometry.
abstract: A liquid chromatography-tandem mass spectrometry method was developed and validated for simultaneous determination of disulfoton and five of its oxidative metabolites (disulfoton-sulfoxide, disulfoton-sulfone, demeton-S, demeton-S-sulfoxide and demeton-S-sulfone) in human whole blood and urine. Extraction was undertaken using a QuEChERS method, which is commonly used in food analysis. D10-Disulfoton was used as the internal standard. Separation was carried out using a CAPCELL-PAK MG II column (35×2.0 mm i.d., 5 μm, Shiseido) with a mobile phase of 10 m mol/L ammonium formate and methanol. This method was applied in an autopsy case, and disulfoton and its oxidative metabolites were successfully detected in both blood and urine. The concentrations of disulfoton in the blood and urine were 360 and 23.8 ng/mL, respectively. There was a relatively low concentration of demeton-S in both the blood (4.0 ng/mL) and urine (45.7 ng/mL). To date, there have been no reported cases of detection of demeton-S in human samples.
authors: Division of Forensic Medicine, Department of Public Health and Forensic Medicine, Tohoku University Graduate School of Medicine, Sendai 980-8575, Japan. usui@forensic.med.tohoku.ac.jp
authors: Kiyotaka
authors: K
authors: Usui
authors: Yoshie
authors: Y
authors: Hayashizaki
authors: Takashi
authors: T
authors: Minagawa
authors: Masaki
authors: M
authors: Hashiyada
authors: Anri
authors: A
authors: Nakano
authors: Masato
authors: M
authors: Funayama
mesh_terms: D000368:Aged; D002853:Chromatography, Liquid; D004222:Disulfoton / Q000097:blood* / Q000652:urine*; D006801:Humans; D007306:Insecticides / Q000097:blood / Q000652:urine; D008297:Male; D013405:Suicide; D053719:Tandem Mass Spectrometry / Q000379:methods
chemical_list: D007306:Insecticides; D004222:Disulfoton