Optimization of acquisition and processing times for the measurement of ¹H to ¹³C polarization transfer kinetics

Solid-state NMR (ssNMR) is a unique technique allowing the study of macromolecular assemblies in their native state without prior modification. The proposed method simplifies the current long and tedious data-acquisition and processing protocols for Variable Contact Time (VCT) ssNMR experiments used in dynamic studies of macromolecular assemblies. Using cellulose nanocrystals as a model for polysaccharide assembly, the acquisition time was reduced by decreasing the number of scans and shortening the recycling time required for the ¹H to ¹³C polarization transfers.•A tenfold reduction in the acquisition time for each kinetic point was achieved while maintaining a good signal to noise ratio.•The processing time for the pseudo-2D solid-state NMR data was also shortened by using signal intensities derived from peak picking rather than the classically-used spectral deconvolution method.•These optimizations enabled the molecular dynamic parameters T_1ρ ^H, T_HH, T_CH to be accessed within a day.