title: Gas chromatography-ion trap mass spectrometry method for the simultaneous measurement of MDMA (ecstasy) and its metabolites, MDA, HMA, and HMMA in plasma and urine.
abstract: The investigation of 3,4-methylenedioxymethamphetamine (MDMA; ecstasy) abuse requires very robust methods with high sensitivity and wide linearity ranges for the quantification of this drug of abuse and its main metabolites in body fluids. An optimized gas chromatography-ion trap mass spectrometry (GC-IT/MS) methodology with electron impact ionization addressing these issues is presented. The sample preparation involves an enzymatic hydrolysis of urine and plasma for conjugate cleavage, a SPE extraction, and a derivatization process. The method was fully validated in rat plasma and urine. Linearity for a wide concentration range was achieved for MDMA, and the metabolites 3,4-methylenedioxyamphetamine (MDA), 4-hydroxy-3-methoxyamphetamine (HMA) and 4-hydroxy-3-methoxymethamphetamine (HMMA). Limits of quantification were 2 ng/mL in plasma and 3.5 ng/mL in urine using a Selected Ion Monitoring detection mode. Selectivity, accuracy, precision, and recovery met the required criteria for the method validation. This GC-IT/MS method provides high sensitivity and adequate performance characteristics for the simultaneous quantification of MDMA, MDA, HMA and HMMA in the studied matrices.
authors.affiliation: REQUIMTE, Toxicology Department, Faculty of Pharmacy, University of Porto, Rua Aníbal Cunha 164, 4099-030 Porto, Portugal.
authors.forename: Daniel Gomes
authors.initials: DG
authors.lastname: da Silva
authors.forename: Paula Guedes
authors.initials: PG
authors.lastname: de Pinho
authors.forename: Helena
authors.initials: H
authors.lastname: Pontes
authors.forename: Luísa
authors.initials: L
authors.lastname: Ferreira
authors.forename: Paula
authors.initials: P
authors.lastname: Branco
authors.forename: Fernando
authors.initials: F
authors.lastname: Remião
authors.forename: Félix
authors.initials: F
authors.lastname: Carvalho
authors.forename: M Lurdes
authors.initials: ML
authors.lastname: Bastos
authors.forename: Helena
authors.initials: H
authors.lastname: Carmo
mesh_terms: D015104:3,4-Methylenedioxyamphetamine / Q000032:analysis* / Q000097:blood / Q000652:urine; D000818:Animals; D004298:Dopamine / Q000031:analogs & derivatives* / Q000032:analysis / Q000097:blood / Q000652:urine; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D008297:Male; D008694:Methamphetamine / Q000031:analogs & derivatives* / Q000032:analysis / Q000097:blood / Q000652:urine; D018817:N-Methyl-3,4-methylenedioxyamphetamine / Q000097:blood / Q000378:metabolism* / Q000652:urine; D051381:Rats; D017208:Rats, Wistar; D012680:Sensitivity and Specificity
chemical_list: C079646:4-hydroxy-3-methoxymethamphetamine; C031105:3-O-methyl-alpha-methyldopamine; D008694:Methamphetamine; D015104:3,4-Methylenedioxyamphetamine; D018817:N-Methyl-3,4-methylenedioxyamphetamine; D004298:Dopamine