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Laboratory of Toxicology and
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Laboratory of Medicinal Chemistry, Ghent University, Harelbekestraat 72, B-9000 Gent, Belgium.
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Laboratory of Forensic Medicine, Ghent University, J.
Kluyskensstraat 29, B-9000 Gent, Belgium.
a Author for correspondence. Fax 32-9-264-81-97; e-mail
Andre.DeLeenheer{at}rug.ac.be
Background: The popular designer drugs 3,4-methylenedioxymethamphetamine (MDMA) and 3,4-methylenedioxyethylamphetamine (MDEA) can be determined in serum, whole blood, and urine, but also in vitreous humor. The latter matrix is interesting when dealing with decomposed bodies in a toxicological setting.
Methods: After extraction, chromatographic separation was achieved on a narrow-bore C18 column by gradient elution with fluorometric detection; results were confirmed by liquid chromatography-tandem mass spectrometry (LC-MS/MS).
Results: The method was linear over the range of 21000 µg/L for whole blood, serum, and vitreous humor, and 0.15 mg/L for urine. Extraction recoveries were >70%, imprecision (CV) was 2.519%, and analytical recoveries were 95.5104.4%. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.8 and 2 µg/L, respectively, for whole blood, serum, and vitreous humor, and 2.5 µg/L and 0.1 mg/L, respectively, for urine. Excellent correlations between the quantitative LC-fluorescence and LC-MS/MS results were obtained. We found the following concentrations in a thanatochemical distribution study in rabbits: in serum, 5.3685 µg/L for MDMA and from the LOQ to 14.5 µg/L for 3,4-methylenedioxyamphetamine (MDA); in whole blood, 19.7710 µg/L for MDMA and from the LOQ to 17.8 µg/L for MDA; in vitreous humor, 12.197.8 µg/L for MDMA and from the LOQ to 3.86 µg/L for MDA. In routine toxicological urine samples, concentrations ranged from LOQ to 14.62 mg/L for MDA, from LOQ to 157 mg/L for MDMA, and from LOQ to 32.54 mg/L for MDEA.
Conclusions: The HPLC method described is sensitive, specific, and suitable for the determination of MDMA, MDEA, and MDA in whole blood, serum, vitreous humor, and urine.
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S. O. Pirnay, T. T. Abraham, and M. A. Huestis Sensitive Gas Chromatography-Mass Spectrometry Method for Simultaneous Measurement of MDEA, MDMA, and Metabolites HMA, MDA, and HMMA in Human Urine Clin. Chem., September 1, 2006; 52(9): 1728 - 1734. [Abstract] [Full Text] [PDF] |
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