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13C-detection two-dimensional NMR approaches for cellulose derivatives

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Abstract

To demonstrate the effectiveness of 13C-detection two-dimensional NMR methods used for the characterization protein structures for the characterization of cellulose derivatives, 13C–13C COSY, 13C–13C INADEQUATE, and 13C–13C TOCSY experiments were applied to 13C-enriched sodium carboxymethyl cellulose and cellulose acetate. These samples were prepared from bacterial cellulose biosynthesized by Gluconacetobacter xylinus ATCC 53582 in medium containing 20 % uniformly 13C-labelled glucose in unlabeled glucose. The combination of 13C–13C COSY (or 13C–13C INADEQUATE) and 13C–13C TOCSY spectra of the cellulose derivatives facilitated the direct and precise assignment of all ring carbons of each anhydroglucose unit comprising the cellulose chain during the short experimental time. In addition, a short spin-lock time (~24 ms) in the 13C–13C TOCSY experiments was revealed to be preferable for achieving improved sensitivity and obtaining correlation signals between all carbons in the anhydroglucose units of the cellulose derivatives.

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Abbreviations

13C:

Carbon-13

15N:

Nitrogen-15

1D:

One-dimensional

1H:

Proton

2D:

Two-dimensional

AGU:

Anhydroglucose unit

BC:

Bacterial cellulose

CA:

Cellulose acetate

CMC:

Carboxymethyl cellulose sodium salt

COSY:

Correlation spectroscopy

D2O:

Deuterium oxide

DIPSI:

Decoupling in the presence of scalar interactions

DMSO:

Dimethyl sulfoxide

DQ:

Double quantum

DSAC :

Substitution degree of acetyl group

DSCM :

Substitution degree of carboxymethyl group

DSS:

4,4-Dimethyl-4-silapentane-1-sulfonic acid

FID:

Free induction decay

G. xylinus :

Gluconacetobacter xylinus

HSQC:

Heteronuclear single quantum coherence

INADEQUATE:

Incredible natural abundance double quantum transfer experiment

NMR:

Nuclear magnetic resonance

NOESY:

Nuclear Overhauser and effect spectroscopy

S/N:

Signal-to-noise ratio

SQ:

Single quantum

T 2 :

Spin–spin relaxation time

TOCSY:

Total correlation spectroscopy

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Acknowledgments

This work was supported in part by Grants-in-Aid for Scientific Research C-25410134 from the Japan Society for Promotion of Science (JSPS).

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Authors and Affiliations

  1. Department of Science and Engineering for Materials, Tomakomai National College of Technology, Nishikioka 443, Tomakomai, Hokkaido, 059 1275, Japan

    Hiroyuki Kono, Hikaru Anai, Hisaho Hashimoto & Yuuichi Shimizu

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  1. Hiroyuki Kono
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  2. Hikaru Anai
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  3. Hisaho Hashimoto
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  4. Yuuichi Shimizu
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Correspondence to Hiroyuki Kono.

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Kono, H., Anai, H., Hashimoto, H. et al. 13C-detection two-dimensional NMR approaches for cellulose derivatives. Cellulose 22, 2927–2942 (2015). https://doi.org/10.1007/s10570-015-0697-9

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