Routine analysis of amphetamine and methamphetamine in biological materials by gas chromatography-mass spectrometry and on-column derivatization.
A simple determination method of amphetamine (AP) and methamphetamine (MA) in biological materials was developed using on-column derivatization and gas chromatography-mass spectrometry (GC-MS). AP and MA in biological materials were adsorbed on the surface of Extrelut and then extracted and derivatized simultaneously on the Extrelut column. AP and MA were derivatized to the N-propoxycarbonyl derivatives using propylchloroformate. Pentadeuterated MA was used as an internal standard. The recoveries of AP and MA from urine were 88.2 and 92.5%, and those from blood were 89.7 and 90.3%, respectively. The calibration curves showed linearity in the range of 12.5-2000 ng/ml (ng/g) for AP and MA in urine and blood, and 0.25-20 ng/mg in hair. When urine samples containing two different concentrations (200 and 1000 ng/ml) of AP and MA, blood samples containing two different concentrations (200 and 1000 ng/g) of AP and MA, hair samples containing two different concentrations (0.5 and 5.0 ng/mg) of AP and MA, the coefficients of variation of intra-day and inter-day were 0.68-3.60% in urine, 0.42-4.58% in blood, and 1.20-13.1% in hair. Furthermore, this proposed method was applied to a medico-legal case of MA intoxication.
Nishida
Manami
M
Department of Legal Medicine, Graduate School of Biomedical Sciences, Hiroshima University, 1-2-3 Kasumi, Minami-ku, 734-8551, Hiroshima, Japan. nishidam@hiroshima-u.ac.jp
Namera
Akira
A
Yashiki
Mikio
M
Kojima
Tohru
T
D000328:Adult; D000661:Amphetamine / Q000032:analysis* / Q000097:blood / Q000652:urine; D002138:Calibration; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D008297:Male; D008694:Methamphetamine / Q000032:analysis* / Q000097:blood / Q000652:urine; D012015:Reference Standards; D015203:Reproducibility of Results
D008694:Methamphetamine; D000661:Amphetamine