title: Small Molecule Mixture Analysis by Heteronuclear NMR under Spin Diffusion Conditions in Viscous DMSO-Water Solvent.
abstract: 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 2D1H-1H NOESY and1H-13C HSQC-NOESY,1H-15N HSQC-NOESY, 1D and 2D1H-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.
authors.affiliation: Université de Reims Champagne-Ardenne, Institut de Chimie Moléculaire de Reims, CNRS UMR 7312, SFR CAP-Santé BP 1039, 51687, Reims Cedex 02, France.
authors.forename: Pedro
authors.identifier: http://orcid.org/0000-0001-8416-750X
authors.initials: P
authors.lastname: Lameiras
authors.affiliation: Université de Reims Champagne-Ardenne, Institut de Chimie Moléculaire de Reims, CNRS UMR 7312, SFR CAP-Santé BP 1039, 51687, Reims Cedex 02, France.
authors.forename: Solène
authors.initials: S
authors.lastname: Patis
authors.affiliation: Université de Reims Champagne-Ardenne, Institut de Chimie Moléculaire de Reims, CNRS UMR 7312, SFR CAP-Santé BP 1039, 51687, Reims Cedex 02, France.
authors.forename: Jouda
authors.initials: J
authors.lastname: Jakhlal
authors.affiliation: Université de Reims Champagne-Ardenne, Institut de Chimie Moléculaire de Reims, CNRS UMR 7312, SFR CAP-Santé BP 1039, 51687, Reims Cedex 02, France.
authors.forename: Stéphanie
authors.initials: S
authors.lastname: Castex
authors.affiliation: Université de Reims Champagne-Ardenne, Institut de Chimie Moléculaire de Reims, CNRS UMR 7312, SFR CAP-Santé BP 1039, 51687, Reims Cedex 02, France.
authors.forename: Pascale
authors.initials: P
authors.lastname: Clivio
authors.affiliation: Université de Reims Champagne-Ardenne, Institut de Chimie Moléculaire de Reims, CNRS UMR 7312, SFR CAP-Santé BP 1039, 51687, Reims Cedex 02, France.
authors.forename: Jean-Marc
authors.identifier: http://orcid.org/0000-0002-5120-2556
authors.initials: JM
authors.lastname: Nuzillard
keywords: NMR spectroscopy; mixture analysis; spin diffusion; structure elucidation; viscous solvent