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.