Development of enantioselective high-performance liquid chromatography-tandem mass spectrometry method for the quantitative determination of 3,4-methylenedioxy-methamphetamine (MDMA) and its phase-1 metabolites in human biological fluids
Lo Faro, Alfredo (Università Politecnica delle Marche (Roma, Itàlia))
Sprega, Giorgia (Università Politecnica delle Marche (Roma, Itàlia))
Beradinelli, Diletta (Università Politecnica delle Marche (Roma, Itàlia))
Tini, Anstasio (Università Politecnica delle Marche (Roma, Itàlia))
Poyatos, Lourdes (Institut Germans Trias i Pujol)
Papaseit, Esther (Institut Germans Trias i Pujol)
Berretta, Paolo (National Centre on Addiction and Doping. Istituto Superiore di Sanit'a)
Di Giorgi, Alessandro (Istituto Superiore di Sanità (Roma, Itàlia))
Farré Albaladejo, Magí (Institut Germans Trias i Pujol)
Takaishvili, Nino (Tbilisi State University (Gerogia))
Farkas, Tivadar (Phenomenex (Estats Units d'Amèrica))
Busardo, Francesco Paolo (Università Politecnica delle Marche (Roma, Itàlia))
Chankvetadze, Bezhan (Tbilisi State University (Georgia))

Data:	2024
Resum:	In the present study enantioselective high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) methods were developed for the quantitative determination of 3,4-methylenedioxy-methamphetamine (MDMA) and its major phase-1 metabolites 4-hydroxy-3-methoxyamphetamine (HMA), 4-hydroxy-3-methoxymethamphetamine (HMMA) and 3,4-methylenedioxyamphetamine (MDA) in human plasma, sweat, oral fluid (OF) and urine. The simultaneous separation of all these compounds and their respective enantioseparation was accomplished on two polysaccharide-based chiral columns. The Lux AMP column with a proprietary chiral selector enabled baseline separation of the enantiomers of MDMA, HMA and HMMA while MDA enantiomers could not be separated with this column under the experimental conditions used in this study. The Lux i-Amylose-3 column based on amylose tris(5-chloro-3-methylphenylcarbamate) as chiral selector baseline-separated the enantiomers of MDMA, HMMA and MDA while the enantiomers of HMA could not be separated. Thus, the various samples were analyzed by using both columns alternatively in combinations with acetonitrile containing 25% (v/v) 5 mM ammonium bicarbonate buffer at pH 11. 0 as mobile phase. Analysis time was less than 4 min with the Lux AMP column and less than 6 min with the Lux i-Amylose-3 column. Both methods were validated and applied to the enantioselective determination of MDMA and its phase-I metabolites in human biological fluids, and enantioselective metabolism of MDMA was confirmed.
Ajuts:	Instituto de Salud Carlos III PI17/01962 Instituto de Salud Carlos III PI20/00879
Drets:	Aquest document està subjecte a una llicència d'ús Creative Commons. Es permet la reproducció total o parcial, la distribució, la comunicació pública de l'obra i la creació d'obres derivades, fins i tot amb finalitats comercials, sempre i quan es reconegui l'autoria de l'obra original.
Llengua:	Anglès
Document:	Article ; recerca ; Versió publicada
Matèria:	Chiral HPLC ; Enantioselective metabolism ; Enantioseparation MDMA and metabolites
Publicat a:	Journal of Pharmaceutical and Biomedical Analysis, Vol. 238 (20 2024) , p. 115768, ISSN 1873-264X

DOI: 10.1016/j.jpba.2023.115768

14 p, 3.0 MB

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