Published: Journal of Analytical Toxicology, Volume 20, Number 4, July/August 1996, pp. 255-261.

Detection and Quantitation of Amphetamine and Methamphetamine: Electron Impact and Chemical Ionization with Ammonia—Comparative Investigation on Shimadzu QP 5000 GC–MS System
P. Dallakian, H. Budzikiewicz, and H. Brzezinka

Gas chromatographic–mass spectrometric (GC–MS) analyses of amphetamine and methamphetamine with chemical ionization (CI) (NH₃) and electron impact (EI) were compared after solid-phase extraction from urine. The optimal CI (NH₃) conditions for amphetamines were selected; the CI mass spectra of amphetamine, methamphetamine, methylenedioxyamphetamine (MDA), methylenedioxymethamphetamine (MDMA), and methylenedioxyethylamphetamine (MDEA) were obtained. Amphetamine and methamphetamine were monitored as [M+H]+ ions in SIM mode. Under these conditions the GC–MS limits of detection and quantitation were determined for amphetamine (2.1 and 5.0 mg/L, respectively) and for methamphetamine (0.9 and 2.0 mg/L, respectively). The heptafluorobutanoyl (HFB) derivatives were used to increase the sensitivity of the GC–MS analysis of amphetamines. Under CI (NH₃) conditions these compounds form mainly the cluster ions [M+NH₄]+. For HFB-derivatives the limits of detection and quantitation for CI (NH₃) were 95 and 170 µg/L, respectively, for amphetamine (m/z 349) and 90 and 160 µg/L, respectively, for methamphetamine (m/z 363). For EI they were 10 and 30 µg/L, respectively, for amphetamine (m/z 240) and 9 and 27 µg/L, respectively, for methamphetamine (m/z 254). The GC–MS–CI (NH₃) technique was found to be suitable for confirmation of amphetamine and methamphetamine in urine samples in addition to the routine GC–MS–EI method.

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