Journal of pharmaceutical and biomedical analysis
January 20, 2024
Alfredo Fabrizio Lo Faro, Giorgia Sprega, Diletta Beradinelli et al.
14 citations
Enantioselective high-performance liquid chromatography-tandem mass spectrometry methods were developed to quantify MDMA and its phase-1 metabolites HMA, HMMA, and MDA in human plasma, sweat, oral fluid, and urine. Two polysaccharide-based chiral columns achieved baseline separation of most enantiomer pairs: the Lux AMP column separated MDMA, HMA, and HMMA enantiomers but not MDA; the Lux i-Amylose-3 column separated MDMA, HMMA, and MDA enantiomers but not HMA. Analysis took under 4 minutes with one column and under 6 minutes with the other. Both methods were validated and applied to biological fluids, confirming enantioselective metabolism of MDMA.
Journal of pharmaceutical and biomedical analysis
June 15, 2024
Giorgia Sprega, Giorgi Kobidze, Alfredo Fabrizio Lo Faro et al.
4 citations
An improved chiral LC-MS/MS method separates all four pairs of enantiomers of MDMA and its major phase-1 metabolites (HMA, HMMA, MDA) on a single Lux AMP column within six minutes, using an optimized mobile phase and column dimensions. The method was applied to human plasma, oral fluid, and urine. In urine, hydrolysis of glucuronides with hydrochloric acid or glucuronidase was tested to evaluate effects on the concentration and enantiomeric distribution of the hydroxy metabolites HMA and HMMA.
Journal of pharmaceutical and biomedical analysis
June 15, 2025
Melvin R Euerby, Benjamin S Barrett, Andrew Costello et al.
A practical HPLC method using six polysaccharide-based chiral stationary phases with a single polar organic solvent mobile phase separated the enantiomers and regioisomers of 32 novel diphenidine-derived psychoactive substances. The cellulose tris(3-chloro-4-methylphenylcarbamate) coated on silica gave baseline separation for 25 of 26 monosubstituted diphenidines with resolution values above 1.5, and optimum separation for 21 of them (resolution 2.9–22.4). The chiral selector type and the substituent position on the 1-phenyl ring strongly influenced chiral resolution, with 4-position substituents showing greater discrimination than 2-position ones. Enantiomer elution order reversed for 2-methoxphenidine depending on the stationary phase. Analysis of real samples confirmed 2-methoxphenidine and diphenidine were traded as racemates, and common adulterants did not interfere.