Published: Journal of Analytical Toxicology, Volume 21, Number 1, January/February 1997, pp. 59–69.
Determination of Phenylisothiocyanate
Derivatives of Amphetamine and its Analogues in Biological Fluids
by HPLC–APCI-MS or DAD
M.J. Bogusz, M. Kala, and
R.-D. Maier
Amphetamine (A), methamphetamine (MA), methylenedioxyamphetamine (MDA), methylenedioxyethylamphetamine (MDE), and methylenedioxymethamphetamine (MDMA), as well as eight other sympathomimetic amines (benzyl-1-phenylethylamine, ephedrine, fenfluramine, norfenfluramine, phentermine, phenylethylamine, phenylpropanolamine, and propylhexedrine), were extracted from serum or urine with ether, derivatized with phenylisothiocyanate, and subjected to high-performance liquid chromatographic (HPLC) examination in isocratic mode. Two detection arts were applied: atmospheric pressure chemical ionization (APCI) mass spectrometry (MS) and UV-spectrometry as diode array detection (DAD) or single wavelength at 250 nm. The derivatives were well-separated and showed good chromatographic behavior. Full-scan mass spectra of drugs examined by means of APCI with collision induced dissociation (APCID) contained protonated molecular ions (M+H)+ and fragments typical for particular drugs. APCID-liquid chromatography–mass spectrometry (LC–MS) appeared very selective for differentiation of all drugs involved. The quantitation with APCID was performed using selected ion monitoring (SIM) of (M+H)+ ions and selected fragments of drugs involved and their deuterated analogues. The limits of detection ranged from 0.001 mg/L (MA, MDMA, and MDE) to 0.005 mg/L (A and MDA). In HPLC–DAD, the spectra of MDMA and MDE were practically identical with maxima of 236–240 nm. Other amphetamines showed slightly different spectra with maxima of 245–250 nm. The limits of detection in UV detection amounted to 0.01–0.03 mg/L (single wavelength detector at 250 nm) or 0.05–0.1 mg/L (DAD).
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