Small Molecule Mixture Analysis by Heteronuclear NMR under Spin Diffusion Conditions in Viscous DMSO–Water Solvent

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 sp...

Full description

Saved in:
Bibliographic Details
Published in:Chemistry : a European journal 2017-04, Vol.23 (20), p.4923-4928
Main Authors: Lameiras, Pedro, Patis, Solène, Jakhlal, Jouda, Castex, Stéphanie, Clivio, Pascale, Nuzillard, Jean‐Marc
Format: Article
Language:English
Subjects:
Analytical chemistry
Chemical Sciences
Chemistry
Cross relaxation
Diffusion
Exchange
Magnetization
mixture analysis
NMR spectroscopy
Nuclear magnetic resonance
Solvents
Spectra
spin diffusion
structure elucidation
Tumbling
viscous solvent
Citations: Items that this one cites
Items that cite this one
Online Access:Get full text
Tags: Add Tag
No Tags, Be the first to tag this record!
Description
Summary: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/H2O offers a wide range of potential applications for polar and moderately apolar mixture analysis. In addition to 2D 1H‐1H NOESY and 1H‐13C HSQC‐NOESY, 1H‐15N HSQC‐NOESY, 1D and 2D 1H‐19F 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/H2O (7:3 v/v) and that of a medium‐polarity fluorinated dinucleotide dissolved in [D6]DMSO/H2O (8:2 v/v) by means of spin diffusion in NOESY, HOESY, and HSQC–NOESY experiments. Composite DMSO–water viscous solvents were used for the first time to access the individual NMR spectra of mixture components in spin diffusion conditions. The involvement of heteronuclei such as 19F, 15N, and 13C facilitated spectral interpretation.
ISSN:0947-6539
1521-3765
DOI:10.1002/chem.201700636