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Small Molecule Mixture Analysis by Heteronuclear NMR under Spin Diffusion Conditions in Viscous DMSO–Water Solvent
Author(s) -
Lameiras Pedro,
Patis Solène,
Jakhlal Jouda,
Castex Stéphanie,
Clivio Pascale,
Nuzillard JeanMarc
Publication year - 2017
Publication title -
chemistry – a european journal
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.687
H-Index - 242
eISSN - 1521-3765
pISSN - 0947-6539
DOI - 10.1002/chem.201700636
Subject(s) - heteronuclear molecule , two dimensional nuclear magnetic resonance spectroscopy , chemistry , heteronuclear single quantum coherence spectroscopy , nuclear overhauser effect , spin diffusion , molecule , solvent , analytical chemistry (journal) , proton nmr , nuclear magnetic resonance spectroscopy , diffusion , nuclear magnetic resonance , stereochemistry , organic chemistry , thermodynamics , physics
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 [D 6 ]DMSO/H 2 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 [D 6 ]DMSO/H 2 O (7:3 v/v) and that of a medium‐polarity fluorinated dinucleotide dissolved in [D 6 ]DMSO/H 2 O (8:2 v/v) by means of spin diffusion in NOESY, HOESY, and HSQC–NOESY experiments.