title: Miniaturized sample preparation method for determination of amphetamines in urine.
abstract: A simple and miniaturized sample preparation method for determination of amphetamines in urine was developed using on-column derivatization and gas chromatography-mass spectrometry (GC-MS). Urine was directly applied to the extraction column that was pre-packed with Extrelut and sodium carbonate. Amphetamine (AP) and methamphetamine (MA) in urine were adsorbed on the surface of Extrelut. AP and MA were then converted to a free base and derivatized to N-propoxycarbonyl derivatives using propylchloroformate on the column. Pentadeuterated MA was used as an internal standard. The recoveries of AP and MA from urine were 100 and 102%, respectively. The calibration curves showed linearity in the range of 0.50-50 microg/mL for AP and MA in urine. When urine samples containing two different concentrations (0.50 and 5.0 microg/mL) of AP and MA were determined, the intra-day and inter-day coefficients of variation were 1.4-7.7%. This method was applied to 14 medico-legal cases of MA intoxication. The results were compared and a good agreement was obtained with a HPLC method.
authors.affiliation: Department of Legal Medicine, Graduate School of Biomedical Sciences, Hiroshima University, 1-2-3 Kasumi, Minami-ku, 734-8551, Japan. nishidam@hiroshima-u.ac.jp
authors.forename: Manami
authors.initials: M
authors.lastname: Nishida
authors.forename: Akira
authors.initials: A
authors.lastname: Namera
authors.forename: Mikio
authors.initials: M
authors.lastname: Yashiki
authors.forename: Kojiro
authors.initials: K
authors.lastname: Kimura
mesh_terms: D000662:Amphetamines / Q000506:poisoning / Q000652:urine*; D002254:Carbonates; D000697:Central Nervous System Stimulants / Q000506:poisoning / Q000652:urine*; D007692:Diatomaceous Earth; D005554:Forensic Medicine / Q000379:methods*; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D008297:Male; D008694:Methamphetamine / Q000506:poisoning / Q000652:urine*; D015203:Reproducibility of Results; D012997:Solvents; D015813:Substance Abuse Detection / Q000379:methods*
chemical_list: D000662:Amphetamines; D002254:Carbonates; D000697:Central Nervous System Stimulants; D012997:Solvents; D008694:Methamphetamine; C005686:sodium carbonate; D007692:Diatomaceous Earth; C018540:Extrelut