Determination of MDMA and its Metabolites in Blood and Urine by Gas Chromatography–Mass Spectrometry and Analysis of Enantiomers by Capillary Electrophoresis

Authors: Segura J.¹; Pizarro N.²; Camí J.¹; Ortuño J.²; de la Torre R.³; Farré M.⁴; Hernández-López C.²; Pujadas M.²; Llebaria A.⁵; Joglar J.⁵; Roset P.N.²; Mas M.²

Source: Journal of Analytical Toxicology, Volume 26, Number 3, April 2002 , pp. 157-165(9)

Publisher: Preston Publications

Abstract:

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--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.

Language: English

Document Type:

Affiliations: 1: Pharmacology Research Unit, Institut Municipal d'Investigació Mèdica (IMIM), Universitat Pompeu Fabra 2: Pharmacology Research Unit, Institut Municipal d'Investigació Mèdica (IMIM) 3: Pharmacology Research Unit, Institut Municipal d'Investigació Mèdica (IMIM), Universitat Autònoma, Universitat Pompeu Fabra, Correspondence Address: Pharmacology Research Unit, Institut Municipal d'Investigació Mèdica (IMIM), Doctor Aiguader 80, E-08003 Barcelona, Spain. E-mail: rtorre@imim.es 4: Pharmacology Research Unit, Institut Municipal d'Investigació Mèdica (IMIM), Universitat Autònoma 5: Department of Biological Organic Chemistry, Institut de Investigacions Químiques i Ambientals, E-08003 Barcelona, Spain

Publication date: 2002-04-01

• The Journal of Analytical Toxicology (JAT), established in 1977 and published 9 times a year, is the international source covering a broad range of clinical, forensic, and industrial laboratory topics regarding the isolation, identification, and quantitation of potentially toxic substances.

  With an emphasis on practical application, JAT articles provide improved and novel techniques for use in clinical, forensic, workplace, sports testing (doping), and other toxicology laboratories. Articles describe newly developed methods in immunoassay testing, gas chromatography, liquid chromatography, mass spectrometry, atomic absorption spectrometry, solid and liquid phase extraction techniques, and other analytical approaches. Worldwide readership includes toxicologists, pathologists, chemists, clinicians, researchers, and educators working in medical examiner and law enforcement laboratories, hospitals, university and independent analytical laboratories, as well as the drug manufacturing industry.

  Each year in October, we publish a special issue from the Society of Forensic Toxicologists.

  JAT, as determined by ISI Citation Index, is one of the two most referenced international journals in forensic science.

• Subscribe to this Title
• ingentaconnect is not responsible for the content or availability of external websites

• In this: publication
• By this: publisher
• In this Subject: Ecology ,  Toxicology
• By this author: Segura J. ;  Pizarro N. ;  Camí J. ;  Ortuño J. ;  de la Torre R. ;  Farré M. ;  Hernández-López C. ;  Pujadas M. ;  Llebaria A. ;  Joglar J. ;  Roset P.N. ;  Mas M.

Website © Publishing Technology. Article copyright remains with the publisher, society or author(s) as specified within the article.

• Terms and conditions
• Privacy policy
• Information for advertisers