Small Molecule Mixture Analysis by Heteronuclear NMR under Spin Diffusion Conditions in Viscous DMSO-Water Solvent.
Fiche publication
Date publication
février 2017
Journal
Chemistry (Weinheim an der Bergstrasse, Germany)
Auteurs
Membres identifiés du Cancéropôle Est :
Dr NUZILLARD Jean-Marc
Tous les auteurs :
Lameiras P, Patis S, Jakhlal J, Castex S, Clivio P, Nuzillard JM
Lien Pubmed
Résumé
Spin diffusion in NMR occurs for small- and medium-sized molecules when their tumbling rate reduces in solution so that magnetization exchange by longitudinal cross relaxation becomes highly efficient. Composite DMSO-water viscous solvents were used for the first time to access the individual NMR spectra of a mixture components in spin diffusion conditions. The easy handling and high dissolution power of [D6 ]DMSO/H2 O offers a wide range of potential applications for polar and moderately apolar mixture analysis. In addition to 2D (1) H-(1) H NOESY and (1) H-(13) C HSQC-NOESY, (1) H-(15) N HSQC-NOESY, 1D and 2D (1) H-(19) F heteronuclear NOESY (HOESY) experiments were set up to offer new ways to individualize molecules within a mixture. This article reports the analysis of a polar mixture of four dipeptides dissolved in [D6 ]DMSO/H2 O (7:3 v/v) and that of a medium-polarity fluorinated dinucleotide dissolved in [D6 ]DMSO/H2 O (8:2 v/v) by means of spin diffusion in NOESY, HOESY, and HSQC-NOESY experiments.
Mots clés
NMR spectroscopy, mixture analysis, spin diffusion, structure elucidation, viscous solvent
Référence
Chemistry. 2017 Feb;: