Comprehensive Signal Assignment of 13C‑Labeled Lignocellulose Using Multidimensional Solution NMR and 13C Chemical Shift Comparison with Solid-State NMR
journal contributionposted on 17.09.2013, 00:00 by Takanori Komatsu, Jun Kikuchi
A multidimensional solution NMR method has been developed using various pulse programs including HCCH-COSY and 13C-HSQC-NOESY for the structural characterization of commercially available 13C labeled lignocellulose from potatoes (Solanum tuberosum L.), chicory (Cichorium intybus), and corn (Zea mays). This new method allowed for 119 of the signals in the 13C-HSQC spectrum of lignocelluloses to be assigned and was successfully used to characterize the structures of lignocellulose samples from three plants in terms of their xylan and xyloglucan structures, which are the major hemicelluloses in angiosperm. Furthermore, this new method provided greater insight into fine structures of lignin by providing a high resolution to the aromatic signals of the β-aryl ether and resinol moieties, as well as the diastereomeric signals of the β-aryl ether. Finally, the 13C chemical shifts assigned in this study were compared with those from solid-state NMR and indicated the presence of heterogeneous dynamics in the polysaccharides where rigid cellulose and mobile hemicelluloses moieties existed together.