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. 2013 Apr;74(2):328-38.
doi: 10.1111/tpj.12124. Epub 2013 Mar 4.

Universal fractionation of lignin-carbohydrate complexes (LCCs) from lignocellulosic biomass: an example using spruce wood

Xueyu Du  1 , Goran Gellerstedt, Jiebing Li
Affiliations

Universal fractionation of lignin-carbohydrate complexes (LCCs) from lignocellulosic biomass: an example using spruce wood

Xueyu Du et al. Plant J. 2013 Apr.

Abstract

It is of both theoretical and practical importance to develop a universally applicable approach for the fractionation and sensitive lignin characterization of lignin-carbohydrate complexes (LCCs) from all types of lignocellulosic biomass, both natively and after various types of processing. In the present study, a previously reported fractionation approach that is applicable for eucalyptus (hardwood) and flax (non-wood) was further improved by introducing an additional step of barium hydroxide precipitation to isolate the mannan-enriched LCC (glucomannan-lignin, GML), in order to suit softwood species as well. Spruce wood was used as the softwood sample. As indicated by the recovery yield and composition analysis, all of the lignin was recovered in three LCC fractions: a glucan-enriched fraction (glucan-lignin, GL), a mannan-enriched fraction (GML) and a xylan-enriched fraction (xylan-lignin, XL). All of the LCCs had high molecular masses and were insoluble or barely soluble in a dioxane/water solution. Carbohydrate and lignin signals were observed in (1) H NMR, (13) C CP-MAS NMR and normal- or high-sensitivity 2D HSQC NMR analyses. The carbohydrate and lignin constituents in each LCC fraction are therefore believed to be chemically bonded rather than physically mixed with one another. The three LCC fractions were found to be distinctly different from each other in terms of their lignin structures, as revealed by highly sensitive analyses by thioacidolysis-GC, thioacidolysis-SEC and pyrolysis-GC.

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Figures

Figure 1
Figure 1
Flow chart of the universally applicable LCC fractionation approach (GL, glucan-lignin; GML, glucomannan-lignin; XL, xylanlignin).
Figure 2
Figure 2
Alkaline SEC analysis of spruce LCC fractions (GL, glucan-lignin; GML, glucomannan-lignin; XL, xylan-lignin).
Figure 3
Figure 3
2D HSQC NMR spectrum of xylan-lignin (XL).
Figure 4
Figure 4
2D HSQC NMR spectrum of acetylated glucan-lignin (Ac-GL). A small amount of undeuterated CHCl3 from the CDCl3 solvent was also observed, as indicated.
Figure 5
Figure 5
1H-NMR spectrum of acetylated glucan-lignin (Ac-GL).
Figure 6
Figure 6
13C CP-MAS NMR spectra comparing lignin-free glucomannan and glucomannan-lignin (GML).
Figure 7
Figure 7
2D HSQC NMR spectrum of acetylated glucomannan- lignin (Ac-GML).
Figure 8
Figure 8
Thioacidolysis-SEC chromatograms of spruce LCC fractions (GL, glucan-lignin; GML, glucomannan-lignin; XL, xylan-lignin).
Figure 9
Figure 9
Pyrolysis-GC/MS chromatogram of glucomannan-lignin (GML).
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