Published:Journal of Chromatographic Science,
ISSN 0021-9665Volume
40, Number 1, January 2002, pp. 19-25
Automated Headspace Solid-Phase Microextraction and In-Matrix
Derivatization for the Determination of Amphetamine-Related Drugs in Human Urine
by Gas Chromatography–Mass Spectrometry
Akira Namera*, Mikio Yashiki,
and Tohru Kojima
Department of Legal Medicine, Hiroshima University, Faculty of Medicine, 1-2-3
Kasumi, Minami-ku, Hiroshima 734-8551, Japan
Makoto Ueki
Doping Control Laboratory, Mitsubishi Kagaku Bio-Clinical Labs, 3-30-1 Shimura,
Itabashi-ku, Tokyo 174-8555, Japan
An automated extraction and determination method for the gas
chromatography (GC)–mass spectrometry (MS) analysis of amphetamine-related
drugs in human urine is developed using headspace solid-phase microextraction
(SPME) and in-matrix derivatization. A urine sample (0.5 mL), potassium carbonate
(5M, 1.0 mL), sodium chloride (0.5 g), and ethylchloroformate (20 µL)
are put in a sample vial. Amphetamine-related drugs are converted to ethylformate
derivatives (carbamates) in the vial because amphetamine-related drugs in urine
are quickly reacted with ethylchloroformate. An SPME fiber is then exposed at
80°C for 15 min in the headspace of the vial. The extracted derivatives
to the fiber are desorbed by exposing the fiber in the injection port of a GC–MS.
The calibration curves show linearity in the range of 1.0 to 1000 ng/mL for
methamphetamine, fenfluramine, and methylenedioxymethamphetamine; 2.0 to 1000
ng/mL for amphetamine and phentermine; 5.0 to 1000 ng/mL for methylenedioxyamphetamine;
10 to 1000 ng/mL for phenethylamine; and 50 to 1000 ng/mL for 4-bromo-2,5-dimethoxyphenethylamine
in urine. No interferences are found, and the time for analysis is 30 min for
one sample. Furthermore, this proposed method is applied to some clinical and
medico-legal cases by taking methamphetamine. Methamphetamine and its metabolite
amphetamine are detected in the urine samples collected from the patients involved
in the clinical cases. Methamphetamine, amphetamine, and phenethylamine are
detected in the urine sample collected from the victim of a medico-legal case.
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