PMID- 38430614
OWN - NLM
STAT- MEDLINE
DCOM- 20240408
LR  - 20240408
IS  - 1873-264X (Electronic)
IS  - 0731-7085 (Linking)
VI  - 243
DP  - 2024 Jun 15
TI  - Optimization 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.
PG  - 116076
LID - S0731-7085(24)00116-X [pii]
LID - 10.1016/j.jpba.2024.116076 [doi]
AB  - Recently we published in this journal an enantioselective high-performance liquid 
      chromatography-tandem mass spectrometry (LC-MS/MS) method for the quantitative 
      determination of 3,4-methylenedioxymethamphetamine (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 and urine. Since we did not achieve 
      simultaneous enantioseparation of all 4 compounds with a single chiral column, 
      two amylose-based chiral columns were used alternatively. Further optimization of 
      the mobile phase in the present study enabled baseline separation of all four 
      pairs of enantiomers on a single Lux AMP column. In addition, by optimization of 
      the column dimension and applied flow-rate it became possible to complete the 
      separation within 6 minutes. These new methods were applied to the analysis of 
      human plasma, oral fluid and urine. While results on the concentration of MDMA 
      and its metabolites in various biological fluids were reported in our recent 
      publication, in the present study an attempt was made to hydrolyze glucuronides 
      in urine samples by using alternatively, hydrochloric acid or glucuronidase and 
      to evaluate the effect of hydrolysis on the concentration and enantiomeric 
      distribution of hydroxy metabolites of MDMA such as HMA and HMMA.
CI  - Copyright (c) 2024 The Authors. Published by Elsevier B.V. All rights reserved.
FAU - Sprega, Giorgia
AU  - Sprega G
AD  - Department of Excellence-Biomedical Sciences and Public Health, Universita 
      Politecnica delle Marche, Ancona 60121, Italy.
FAU - Kobidze, Giorgi
AU  - Kobidze G
AD  - Department of Excellence-Biomedical Sciences and Public Health, Universita 
      Politecnica delle Marche, Ancona 60121, Italy.
FAU - Lo Faro, Alfredo Fabrizio
AU  - Lo Faro AF
AD  - Department of Excellence-Biomedical Sciences and Public Health, Universita 
      Politecnica delle Marche, Ancona 60121, Italy. Electronic address: 
      a.lofaro@staff.univpm.it.
FAU - Pichini, Simona
AU  - Pichini S
AD  - National Centre on Addiction and Doping, Istituto Superiore di 
      Sanita, Rome, Italy.
FAU - Farkas, Tivadar
AU  - Farkas T
AD  - Phenomenex Inc., 411 Madrid Ave, Torrance, CA 90501, USA.
FAU - Tini, Anastasio
AU  - Tini A
AD  - Department of Excellence-Biomedical Sciences and Public Health, Universita 
      Politecnica delle Marche, Ancona 60121, Italy.
FAU - Mskhiladze, Antonina
AU  - Mskhiladze A
AD  - Faculty of Natural Sciences, Mathematics, Technologies and Pharmacy, Sokhumi 
      State University, Polytkovskaya 61, Tbilisi 0186, Georgia.
FAU - Busardo, Francesco Paolo
AU  - Busardo FP
AD  - Department of Excellence-Biomedical Sciences and Public Health, Universita 
      Politecnica delle Marche, Ancona 60121, Italy.
FAU - Chankvetadze, Bezhan
AU  - Chankvetadze B
AD  - Institute of Physical and Analytical Chemistry, School of Exact and Natural 
      Sciences, Tbilisi State University, I. Chavchavadze Ave 1, Tbilisi 0179, Georgia.
LA  - eng
PT  - Journal Article
DEP - 20240227
PL  - England
TA  - J Pharm Biomed Anal
JT  - Journal of pharmaceutical and biomedical analysis
JID - 8309336
RN  - KE1SEN21RM (N-Methyl-3,4-methylenedioxyamphetamine)
RN  - 515-30-0 (atrolactic acid)
RN  - 44RAL3456C (Methamphetamine)
RN  - 4764-17-4 (3,4-Methylenedioxyamphetamine)
RN  - 0 (Lactates)
SB  - IM
MH  - Humans
MH  - *N-Methyl-3,4-methylenedioxyamphetamine/urine
MH  - Chromatography, High Pressure Liquid
MH  - Tandem Mass Spectrometry
MH  - Chromatography, Liquid
MH  - Stereoisomerism
MH  - *Methamphetamine
MH  - *3,4-Methylenedioxyamphetamine/urine
MH  - *Lactates
OTO - NOTNLM
OT  - Chiral HPLC
OT  - Enantioselective metabolism
OT  - Enantioseparation
OT  - Hydrolysis of glucuronides
OT  - MDMA and metabolites
COIS- Declaration of Competing Interest The authors declare that they have no known 
      competing financial interests or personal relationships that could have appeared 
      to influence the work reported in this paper.
EDAT- 2024/03/03 17:42
MHDA- 2024/04/08 06:42
CRDT- 2024/03/02 18:02
PHST- 2024/01/03 00:00 [received]
PHST- 2024/02/12 00:00 [revised]
PHST- 2024/02/26 00:00 [accepted]
PHST- 2024/04/08 06:42 [medline]
PHST- 2024/03/03 17:42 [pubmed]
PHST- 2024/03/02 18:02 [entrez]
AID - S0731-7085(24)00116-X [pii]
AID - 10.1016/j.jpba.2024.116076 [doi]
PST - ppublish
SO  - J Pharm Biomed Anal. 2024 Jun 15;243:116076. doi: 10.1016/j.jpba.2024.116076. 
      Epub 2024 Feb 27.