A ¹³C three-dimensional DQ-SQ-SQ correlation experiment for high-resolution analysis of complex carbohydrates using solid-state NMR

J Magn Reson. 2022 Jan 21;336:107148. doi: 10.1016/j.jmr.2022.107148. Online ahead of print.

ABSTRACT

Complex carbohydrates are the key components of the protective cell walls of microbial pathogens and the bioenergy reservoir in plants and algae. Structural characterization of these polymorphic molecules requires assistance from multidimensional ¹³C correlation approaches. To facilitate the analysis of carbohydrate structure using solid-state NMR, we present a three-dimensional (3D) ¹³C-¹³C-¹³C experiment that includes a double-quantum (DQ) dimension and is thus free of the cube’s body diagonal. The enhanced resolution supports the unambiguous resonance assignment of many polysaccharides in plant and fungal cell walls using uniformly ¹³C-labeled cells of spruce and Aspergillus fumigatus. Long-range structural restraints were effectively obtained to revisit our understanding of the spatial organization of plant cellulose microfibrils. The method is widely applicable to the investigations of cellular carbohydrates and carbon-based biomaterials.

PMID:35121490 | DOI:10.1016/j.jmr.2022.107148