Cross-Polarization/Magic-Angle Spinning ^〈13〉C Nuclear Magnetic Resonance Study of Cellulose I-Ethylenediamine Complex

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Complete assignments of the cross-polarization/magic-angle spinning (CP/MAS) ^<13>C nuclear magnetic resonance (NMR) spectrum of the cellulose I-ethylenediamine (EDA) complex, which is the intermediate of the reaction from cellulose I to cellulose III_I, were performed. In this paper, we used the ^<13>C-enriched cellulose that was biosynthesized by Acetobacter xylinum ATCC10245 strain from culture medium containing D- (2-^<13>C), D- (3-^<13>C), or D- (5-^<13>C) glucose as a carbon source. After conversion into cellulose I-EDA complex by sufficient EDA treatment, the CP/MAS ^<13>C NMR spectra of the ^<13>C-enriched cellulose I-EDA complexes were measured. As a result, ^<13>C resonance lines of each carbon of the cellulose moiety in the complex appeared as a singlet, suggesting that all glucose residues of the complex are magnetically equivalent. The difference in chemical shifts for each carbon between cellulose I-EDA and cellulose I_α, I_β, and III_I, respectively, suggests that the conformation of the cellulose chains for cellulose I-EDA differs from that for cellulose I_α, I_β, and III_I. In addition, fitting analysis of the ^<13>C spectrum of Valonia cellulose I-EDA complex revealed that the complex contains one EDA molecule per two glucose residues in the cellulose chain.
社団法人日本生物工学会の論文
2003-11-25