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.
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.
da Silva
Daniel Gomes
DG
REQUIMTE, Toxicology Department, Faculty of Pharmacy, University of Porto, Rua Aníbal Cunha 164, 4099-030 Porto, Portugal.
de Pinho
Paula Guedes
PG
Pontes
Helena
H
Ferreira
Luísa
L
Branco
Paula
P
Remião
Fernando
F
Carvalho
Félix
F
Bastos
M Lurdes
ML
Carmo
Helena
H
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
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