Journal Article

Comparison of Five Derivatizing Agents for the Determination of Amphetamine-Type Stimulants in Human Urine by Extractive Acylation and Gas Chromatography–Mass Spectrometry

Adrienn Dobos, Előd Hidvégi and Gábor Pál Somogyi

in Journal of Analytical Toxicology

Volume 36, issue 5, pages 340-344
Published in print June 2012 | ISSN: 0146-4760
Published online June 2012 | e-ISSN: 1945-2403 | DOI: http://dx.doi.org/10.1093/jat/bks026
Comparison of Five Derivatizing Agents for the Determination of Amphetamine-Type Stimulants in Human Urine by Extractive Acylation and Gas Chromatography–Mass Spectrometry

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Five acylation reagents have been compared for use as derivatizing agents for the analysis of amphetamine-type stimulants (ATS) in urine by gas chromatography–mass spectrometry (GC–MS). The evaluated reagents were heptafluorobutyric anhydride, pentafluoropropionic anhydride, trifluoroacetic anhydride, acetic anhydride (AA) and N-methyl-bis(trifluoroacetamide). The ATS included amphetamine, methamphetamine (MA), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA) and 3,4-methylenedioxyethylamphetamine (MDEA). A mixture of the ATS was added to urine (1 mL) followed by KOH solution and saturated NaHCO3 solution. The sample was then extracted with dichloromethane and the derivatizing agent and 2 µL were injected into the GC–MS instrument. The derivatizing agents were compared with reference to the signal-to-noise (S/N) ratios, peak area values, relative standard deviations (RSDs), linearities, limits of detection (LODs) and selectivities. The acetic anhydride proved to be the best according to the S/N ratio and peak area results for amphetamine, MA, MDMA and MDEA. The best RSD values of peak areas and of S/N ratios at 3 µg/mL were also given by AA in cases of MDA, MDMA and MDEA. At 20 µg/mL, the lowest RSD values of peak areas for MDA and the lowest RSD values of S/N ratios for MA, MDA, MDMA and MDEA were again given by AA. Additionally, the highest correlation coefficients for MA, MDA, MDMA and MDEA and the lowest LOD results for MA, MDMA and MDEA were produced by AA.

Journal Article.  2601 words.  Illustrated.

Subjects: Medical Toxicology ; Toxicology (Non-medical)

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