Journal Article

Determination of Phenylisothiocyanate Derivatives of Amphetamine and its Analogues in Biological Fluids by HPLC-APCI-MS or DAD

Maciej J. Bogusz, Maria Kala and Rolf-Dieter Maier

in Journal of Analytical Toxicology

Volume 21, issue 1, pages 59-69
Published in print January 1997 | ISSN: 0146-4760
Published online January 1997 | e-ISSN: 1945-2403 | DOI: http://dx.doi.org/10.1093/jat/21.1.59
Determination of Phenylisothiocyanate Derivatives of Amphetamine and its Analogues in Biological Fluids by HPLC-APCI-MS or DAD

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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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Subjects: Medical Toxicology ; Toxicology (Non-medical)

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