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Nondestructive Analysis of Lignin Structure by NMR Spectroscopy of Specifically 13C-Enriched Lignins I: Solic State Study of Ginkgo Wood

Published

Author(s)

N Terashima, J Hafren, U Westermark, David L. VanderHart

Abstract

Guaiacyl-type lignin is the major component of ginkgo lignin. Specific 13C-enrichment of alpha, beta and gamma-carbons of the guaiacylpropane side chains was achieved by administration of coniferin-[alpha-13C], coniferin-[beta-13C] and coniferin-[gamma-13C] respectively to growing stems of ginkgo trees. Unenriched coniferin was administered as a control. The xylem tissues containing specifically 13C-enriched lignins or unenriched lignin were subjected to analysis by solid state NMR. Subtraction of the spectrum of tissue containing unenriched lignin from the spectra of tissues containing 13C-enriched lignins gave difference spectra exclusively assigned to the enriched side chain carbons of intact protolignin in the cell walls. From the signal intensities determined under quantitative conditions and an estimate of corresponding standard uncertainties, the percentage ranges of the major inter-unit lignin bonds originating from the beta-carbon of the coniferin precursor were estimated to be: beta-O-4/alpha-O-R (R = H, polysaccharides or lignols) including beta-OH, 53 % to 57 %; combined beta-5, beta-beta and beta-1, 32 % to 36 %; coniferaldehyde end groups, 2 % to 4 %; and coniferyl alcohol end groups, 4 % to 6 %.
Citation
Holzforschung
Volume
56 No. 1

Keywords

C13 enrichment, coniferin, ginkgo, lignin, nmr, protolignin, solid state

Citation

Terashima, N. , Hafren, J. , Westermark, U. and VanderHart, D. (2002), Nondestructive Analysis of Lignin Structure by NMR Spectroscopy of Specifically 13C-Enriched Lignins I: Solic State Study of Ginkgo Wood, Holzforschung, [online], https://tsapps.nist.gov/publication/get_pdf.cfm?pub_id=851728 (Accessed May 26, 2024)

Issues

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Created December 31, 2001, Updated October 12, 2021