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Published:
Journal of Analytical Toxicology,
ISSN 0146-4760,
Volume 26, Number 3, April,
pp. 157-165
Determination of MDMA and its Metabolites in Blood and
Urine by Gas Chromatography–Mass Spectrometry and Analysis of Enantiomers
by Capillary Electrophoresis
Nieves Pizarro[1], Jordi Ortuño[1], Magí
Farré[1],[2], Cándido Hernández-López[1], Mitona
Pujadas[1], Amadeu Llebaria[3], Jesús Joglar[3], Pere N. Roset[1], Marta
Mas[1], Jordi Segura[1],[4], Jordi Camí[1],[4], and Rafael de la Torre[1],[2],[4]
[1]Pharmacology Research Unit, Institut Municipal d’Investigació
Mèdica (IMIM);
[2]Universitat Autònoma and
[4]Universitat Pompeu Fabra; and
[3]Department of Biological Organic Chemistry, Institut de Investigacions Químiques
i Ambientals, E-08003 Barcelona, Spain
A gas chromatography–mass
spectrometry (GC–MS) method was used for the simultaneous quantitation
of 3,4-methylenedioxymethamphetamine (MDMA) and the 3,4-methylenedioxyamphetamine
(MDA), 4-hydroxy-3-methoxymethamphetamine (HMMA), and 4-hydroxy-3-methoxyamphetamine
(HMA) metabolites in plasma and urine samples after the administration of 100
mg MDMA to healthy volunteers. Samples were hydrolyzed prior to a solid-phase
extraction with Bond Elut Certify® columns. Analytes were eluted with ethyl
acetate (2% ammonium hydroxide) and analyzed as their trifluoroacyl derivatives.
Linear calibration curves were obtained at plasma and urine concentration ranges
of 25–400 ng/mL and 250–2000 ng/mL for MDMA and HMMA, and of 2.5–40
ng/mL and 100–1000 ng/mL for MDA and HMA. Following the same urine preparation
procedure but without the derivatization step, a capillary electrophoresis (CE)
method for enantiomerical resolution of compounds was developed using (2-hydroxy)propyl-b-cyclodextrin
at two different concentrations (10 and 50mM in 50mM H3PO4, pH 2.5) as chiral
selector. Calibration curves for the CE method were prepared with the corresponding
racemic mixture and were linear between 125 and 2000 ng/mL, 50 and 1000 ng/mL,
and 125 and 1500 ng/mL for each enantiomer of MDMA, MDA, and HMMA, respectively.
Stereoselective disposition of MDMA and MDA was confirmed. HMMA disposition
seems to be in apparent contradiction with MDMA findings as the enantiomer ratio
is close to 1 and constant over the time. Reproduction
of editorial content of this journal is prohibited without publisher’s
permission.
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