Use of Diethanolamine as a Viscous Solvent for Mixture Analysis by Multidimensional Heteronuclear ViscY NMR Experiments
Author(s) -
Ritchy Leroy,
François Pedinielli,
Gautier Bourbon,
JeanMarc Nuzillard,
Pédro Lameiras
Publication year - 2022
Publication title -
analytical chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 2.117
H-Index - 332
eISSN - 1520-6882
pISSN - 0003-2700
DOI - 10.1021/acs.analchem.2c00536
Subject(s) - heteronuclear molecule , chemistry , two dimensional nuclear magnetic resonance spectroscopy , homonuclear molecule , heteronuclear single quantum coherence spectroscopy , nuclear overhauser effect , diethanolamine , nuclear magnetic resonance spectroscopy , analytical chemistry (journal) , molecule , nuclear magnetic resonance , stereochemistry , organic chemistry , physics
Diethanolamine/DMSO- d 6 as a viscous binary solvent is first reported for the individualization of low-polarity mixture components by multidimensional heteronuclear ViscY 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 1 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- d 6 solvent blend using homonuclear selective 1D, 2D 1 H- 1 H NOESY experiments and heteronuclear 1D, 2D 1 H- 19 F heteronuclear Overhauser effect spectroscopy, 2D 1 H- 19 F, 1 H- 31 P HSQC-NOESY, and 3D 1 H- 19 F- 1 H, 1 H- 31 P- 1 H HSQC-NOESY experiments by taking profit from spin diffusion.
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