Use of Diethanolamine as a Viscous Solvent for Mixture Analysis by Multidimensional Heteronuclear NMR Experiments.

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Date publication

juin 2022

Journal

Analytical chemistry

Auteurs

Membres identifiés du Cancéropôle Est :
Dr NUZILLARD Jean-Marc


Tous les auteurs :
Leroy R, Pedinielli F, Bourbon G, Nuzillard JM, Lameiras P

Résumé

Diethanolamine/DMSO- as a viscous binary solvent is first reported for the individualization of low-polarity mixture components by multidimensional heteronuclear NMR experiments under spin diffusion conditions. Solvent viscosity induces the slowing down of molecular tumbling, hence promoting magnetization transfer by dipolar longitudinal cross-relaxation. As a result, all H nuclei resonances within the same molecule may correlate in a 2D nuclear Overhauser effect spectroscopy (NOESY) spectrum, giving access to mixture analysis. We offer a new way to analyze mixtures by considering 3D heteronuclear heteronuclear single-quantum coherence-NOESY (HSQC-NOESY) experiments under viscous conditions. We state the individualization of four low-polarity chemical compounds dissolved in the diethanolamine/DMSO- solvent blend using homonuclear selective 1D, 2D H-H NOESY experiments and heteronuclear 1D, 2D H-F heteronuclear Overhauser effect spectroscopy, 2D H-F, H-P HSQC-NOESY, and 3D H-F-H, H-P-H HSQC-NOESY experiments by taking profit from spin diffusion.

Référence

Anal Chem. 2022 06 23;: