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/H2 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 [D6 ]DMSO/H2 O (7:3 v/v) and that of a medium-polarity fluorinated dinucleotide dissolved in [D6 ]DMSO/H2 O (8:2 v/v) by means of spin diffusion in NOESY, HOESY, and HSQC-NOESY experiments.
