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Structural Characterization of Lignins from Willow Bark and Wood

Journal Article · · Journal of Agricultural and Food Chemistry

Understanding the chemical structure of lignin in willow bark is an indispensable step to design how to separate its fiber bundles. The whole cell wall and enzyme lignin preparations sequentially isolated from ball-milled bark, inner bark, and wood were comparatively investigated by nuclear magnetic resonance (NMR) spectroscopy and three classical degradative methods, i.e., alkaline nitrobenzene oxidation, derivatization followed by reductive cleavage, and analytical thioacidolysis. All results demonstrated that the guaiacyl (G) units were predominant in the willow bark lignin over syringyl (S) and minor p-hydroxyphenyl (H) units. Moreover, the monomer yields and S/G ratio rose progressively from bark to inner bark and wood, indicating that lignin may be more condensed in bark than in other tissues. Additionally, major interunit linkage substructures (β-aryl ethers, phenylcoumarans, and resinols) together with cinnamyl alcohol end groups were relatively quantitated by two-dimensional NMR spectroscopy. Bark and inner bark were rich in pectins and proteins, which were present in large quantities and also in the enzyme lignin preparations.

Research Organization:
Great Lakes Bioenergy Research Center, Madison, WI (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Biological and Environmental Research (BER) (SC-23)
Grant/Contract Number:
SC0018409
OSTI ID:
1505798
Journal Information:
Journal of Agricultural and Food Chemistry, Journal Name: Journal of Agricultural and Food Chemistry Journal Issue: 28 Vol. 66; ISSN 0021-8561
Publisher:
American Chemical SocietyCopyright Statement
Country of Publication:
United States
Language:
English

References (31)

Catalytic organosolv fractionation of willow wood and wheat straw as pretreatment for enzymatic cellulose hydrolysis journal May 2011
Fast multidimensional NMR by polarization sharing journal January 2007
Characterization of nonderivatized plant cell walls using high-resolution solution-state NMR spectroscopy journal June 2008
Efficacy and Safety of White Willow Bark ( Salix alba ) Extracts: Willow Bark Extract Efficacy and Safety journal May 2015
Lignification in the flax stem: evidence for an unusual lignin in bast fibers journal June 2005
Hydroxycinnamates in lignification journal August 2009
Solution-state 2D NMR of Ball-milled Plant Cell Wall Gels in DMSO-d 6 journal March 2008
Naturally p-Hydroxybenzoylated Lignins in Palms journal February 2015
Production of pulp from Salix viminalis energy crops using the FIRSST process journal July 2010
Willow biomass as feedstock for an integrated multi-product biorefinery journal July 2014
NMR Assignment for Diaryl Ether Structures (4–O–5 Structures) in Pine Wood Lignin journal April 2016
Characterization and Elimination of Undesirable Protein Residues in Plant Cell Wall Materials for Enhancing Lignin Analysis by Solution-State Nuclear Magnetic Resonance Spectroscopy journal November 2017
Morphology and Overall Chemical Characterization of Willow ( Salix sp.) Inner Bark and Wood: Toward Controlled Deconstruction of Willow Biomass journal June 2016
Willow Lignin Oxidation and Depolymerization under Low Cost Ionic Liquid journal May 2016
Compositional Analysis of Lignocellulosic Feedstocks. 1. Review and Description of Methods
  • Sluiter, Justin B.; Ruiz, Raymond O.; Scarlata, Christopher J.
  • Journal of Agricultural and Food Chemistry, Vol. 58, Issue 16, p. 9043-9053 https://doi.org/10.1021/jf1008023
journal August 2010
Syntheses of Lignin-Derived Thioacidolysis Monomers and Their Uses as Quantitation Standards journal January 2012
Chemical Composition of Desert Willow ( Salix psammophila ) Grown in the Kubuqi Desert, Inner Mongolia, China: Bark Extracts Associated with Environmental Adaptability journal December 2013
DFRC Method for Lignin Analysis. 1. New Method for β-Aryl Ether Cleavage:  Lignin Model Studies journal December 1997
The DFRC Method for Lignin Analysis. 2. Monomers from Isolated Lignins journal February 1998
Lignins: Natural polymers from oxidative coupling of 4-hydroxyphenyl- propanoids journal January 2004
Whole plant cell wall characterization using solution-state 2D NMR journal August 2012
Fast preparation of RG-I enriched ultra-low molecular weight pectin by an ultrasound accelerated Fenton process journal April 2017
Solution-state 2D NMR of ball-milled plant cell wall gels in DMSO-d6/pyridine-d5 journal January 2010
A gel-state 2D-NMR method for plant cell wall profiling and analysis: a model study with the amorphous cellulose and xylan from ball-milled cotton linters journal January 2014
The structural changes of lignin and lignin–carbohydrate complexes in corn stover induced by mild sodium hydroxide treatment journal January 2014
Salicylates of Intact Salix myrsinifolia Plantlets Do Not Undergo Rapid Metabolic Turnover journal March 2000
Seasonally dependent formation of protein-storage vacuoles in the inner bark tissues of Salix microstachya journal August 1990
Lignin Biosynthesis journal June 2003
Preparative Thioacidolysis of Spruce Lignin: Isolation and Identification of Main Monomeric Products journal January 1986
Chemical Elucidation of Structurally Diverse Willow Lignins journal November 2015
Can Lignin Be Accurately Measured? journal January 2005

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