Skip to main content
U.S. Department of Energy
Office of Scientific and Technical Information

Hemicellulose Modulates Nanoscale Lignin Architecture in Synthetic Plant Cell Walls

Journal Article · · ACS Nano
 [1];  [2];  [3];  [3];  [2];  [1];  [3]
  1. Univ. of Illinois at Urbana-Champaign, IL (United States)
  2. Aix-Marseille Univ., Marseille (France); Centre National de la Recherche Scientifique (CNRS), Marseille (France); Centrale Méditerranée, Marseille (France); Institut Fresnel, Marseille (France)
  3. Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)

Cellulose, hemicellulose, and lignin─the most abundant biopolymers on Earth─compose the structural matrix of plant biomass, providing renewable resources critical to bioenergy and sustainable materials. Despite their importance, the nanoscale mechanochemical processes underlying lignocellulose assembly during plant secondary cell wall formation remain poorly understood, hindering advancements in biomass conversion technologies. Here, in this study, we synthesize a biomimetic model system comprising cellulose–hemicellulose nanofibrils (CHN) to examine guaiacyl lignin polymerization in a physiologically relevant context. Using advanced nanocharacterization─scattering-type scanning near-field optical microscopy (s-SNOM) with infrared nanospectroscopy coupled to solid-state nuclear magnetic resonance (NMR)─we reveal that hemicellulose presence considerably modulates lignin deposition and alters its interunit bond distribution. Specifically, hemicellulose-rich environments dramatically reduce lignin deposition by approximately 50% and yield highly condensed lignin structures characterized by severely reduced β–O–4′ linkages (<2%) and suppressed β–β′ linkages. Conversely, cellulose-alone scaffolds support notably higher β–O–4′ content (∼10%), resulting in a more uniform nanoscale lignin coating. Our work helps explain how accessible hemicellulose sites, both sterically and chemically, direct radical coupling during lignification, fundamentally reshaping lignin’s nanoscale architecture. These findings deepen our mechanistic understanding of plant cell wall biosynthesis and inform strategies aimed at enhancing biomass deconstruction efficiency for sustainable bioenergy applications.

Research Organization:
Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Biological and Environmental Research (BER)
Grant/Contract Number:
SC0023167; AC05-00OR22725
OSTI ID:
3007925
Journal Information:
ACS Nano, Journal Name: ACS Nano Journal Issue: 47 Vol. 19; ISSN 1936-086X; ISSN 1936-0851
Publisher:
American Chemical Society (ACS)Copyright Statement
Country of Publication:
United States
Language:
English

References (64)

Efficient solid-phase synthesis of acetylated lignin and a comparison of the properties of different modified lignins journal September 2016
Lignin Chemistry: Biosynthetic Study and Structural Characterisation of Coniferyl Alcohol Oligomers Formed In Vitro in a Micellar Environment journal May 2010
Study of Self-Assembly of the Lignin Model Compound on Cellulose Model Substrate journal February 2003
Oxidative Coupling during Lignin Polymerization Is Determined by Unpaired Electron Delocalization within Parent Phenylpropanoid Radicals journal August 1996
Recent progress in the chemistry of wood hemicelluloses journal January 1967
Lignin-hemicellulose complexes restrict enzymatic solubilization of mannan and xylan from dissolving pulp journal September 1998
Unveiling the Structural Heterogeneity of Bamboo Lignin by In Situ HSQC NMR Technique journal June 2012
The DOE Bioenergy Research Centers: History, Operations, and Scientific Output journal August 2015
Bioprospecting lignin biomass into environmentally friendly polymers—Applied perspective to reconcile sustainable circular bioeconomy journal March 2022
Enhanced dielectric contrast in scattering-type scanning near-field optical microscopy journal August 2000
Evaluation of the reproducibility of the synthesis of dehydrogenation polymer models of lignin journal January 1998
Influence of pectins on the solubility and the molar mass distribution of dehydrogenative polymers (DHPs, lignin model compounds) journal July 2001
Characterisation of water-soluble galactoglucomannans from Norway spruce wood and thermomechanical pulp journal May 2003
Xylan as limiting factor in enzymatic hydrolysis of nanocellulose journal February 2013
Robustness of two-step acid hydrolysis procedure for composition analysis of poplar journal September 2016
Identification of 4–O–5-Units in Softwood Lignins via Definitive Lignin Models and NMR journal May 2016
Dehydrogenative Polymerization of Coniferyl Alcohol in Artificial Polysaccharides Matrices: Effects of Xylan on the Polymerization journal May 2015
Nanomechanics and Raman Spectroscopy of in Situ Native Carbohydrate Storage Granules for Enhancing Starch Quality and Lignocellulosic Biomass Production journal February 2020
Nanoscale FTIR and Mechanical Mapping of Plant Cell Walls for Understanding Biomass Deconstruction journal February 2022
Surface Characterization of Populus during Caldicellulosiruptor bescii Growth by TOF-SIMS Analysis journal January 2017
Lignin-Inspired Surface Modification of Nanocellulose by Enzyme-Catalyzed Radical Coupling of Coniferyl Alcohol in Pickering Emulsion journal December 2019
Preserving Aryl Ether Linkages and Higher Yields of Isolated Lignin through Biomass Fibrillation journal December 2019
Enzymatic Polymerization of Coniferyl Alcohol in the Presence of Cyclodextrins journal May 2006
Characterization of Arabinoxylan−Dehydrogenation Polymer (Synthetic Lignin Polymer) Nanoparticles journal March 2007
Nanoscale Structure of the Cell Wall Protecting Cellulose from Enzyme Attack journal February 2011
Synthesis and Characterization of Dehydrogenation Polymers in Gluconacetobacter xylinus Cellulose and Cellulose/Pectin Composite journal January 2003
Accurate and Reproducible Determination of Lignin Molar Mass by Acetobromination journal March 2012
Recovery of Permittivity and Depth from Near-Field Data as a Step toward Infrared Nanotomography journal June 2014
Cellulose–Hemicellulose and Cellulose–Lignin Interactions during Fast Pyrolysis journal January 2015
Opto-nanomechanical spectroscopic material characterization journal August 2015
Growth of the plant cell wall journal November 2005
Tomographic and multimodal scattering-type scanning near-field optical microscopy with peak force tapping mode journal May 2018
Plasticity, elasticity, and adhesion energy of plant cell walls: nanometrology of lignin loss using atomic force microscopy journal March 2017
In situ plant materials hyperspectral imaging by multimodal scattering near-field optical microscopy journal June 2021
Karhunen–Loève treatment to remove noise and facilitate data analysis in sensing, spectroscopy and other applications journal September 2014
Cascade enzymatic cleavage of the β-O-4 linkage in a lignin model compound journal January 2016
On the structure of softwood kraft lignin journal January 2017
Cellulose–hemicellulose interactions at elevated temperatures increase cellulose recalcitrance to biological conversion journal January 2018
Phenolic cross-links: building and de-constructing the plant cell wall journal January 2020
Pure optical contrast in scattering-type scanning near-field microscopy journal April 2001
Performance of visible and mid-infrared scattering-type near-field optical microscopes journal June 2003
Imaging a GaAlAs laser diode in operation using apertureless scanning near-field optical microscopy journal March 1999
Pseudoheterodyne detection for background-free near-field spectroscopy journal September 2006
Comparative Studies of Brown Coal and Lignin. I. Infra-Red Spectra journal March 1960
Absence of branches from xylan in Arabidopsis gux mutants reveals potential for simplification of lignocellulosic biomass journal September 2010
Molecular-level design of alternative media for energy-saving pilot-scale fibrillation of nanocellulose journal September 2024
Modifications in Lignin and Accumulation of Phenolic Glucosides in Poplar Xylem upon Down-regulation of Caffeoyl-Coenzyme A O-Methyltransferase, an Enzyme Involved in Lignin Biosynthesis journal August 2000
Quantitative 13 C NMR Characterization of Milled Wood Lignins Isolated by Different Milling Techniques journal April 2006
Cooperative Regulation of Flavonoid and Lignin Biosynthesis in Plants journal March 2021
Near-field microscopy by elastic light scattering from a tip
  • Keilmann, Fritz; Hillenbrand, Rainer
  • Philosophical Transactions of the Royal Society of London. Series A: Mathematical, Physical and Engineering Sciences, Vol. 362, Issue 1817 https://doi.org/10.1098/rsta.2003.1347
journal April 2004
Identification of Novel Genes in Arabidopsis Involved in Secondary Cell Wall Formation Using Expression Profiling and Reverse Genetics journal June 2005
Hemicelluloses journal June 2010
An Empirical Method for Estimating the Degree of Crystallinity of Native Cellulose Using the X-Ray Diffractometer journal October 1959
Natural genetic variability reduces recalcitrance in poplar journal May 2016
Mathematical models of lignin biosynthesis journal February 2018
Lignin–carbohydrate complexes: properties, applications, analyses, and methods of extraction: a review journal September 2018
Near-field optical microscope based on local perturbation of a diffraction spot journal January 1995
What Factors Control Dimerization of Coniferyl Alcohol? journal November 1999
HSQC-NMR analysis of lignin in woody (Eucalyptus globulus and Picea abies) and non-woody (Agave sisalana) ball-milled plant materials at the gel state 10th EWLP, Stockholm, Sweden, August 25–28, 2008 journal November 2009
New Preparations of Lignin Polymer Models under Conditions that Approximate Cell Wall Lignification. I. Synthesis of Novel Lignin Polymer Models and their Structural Characterization by 13 C NMR journal January 1995
13C NMR Characterization of Guaiacyl, Guaiacyl/Syringyl and Syringyl Dehydrogenation Polymers journal January 1998
Nanometrology of Biomass for Bioenergy: The Role of Atomic Force Microscopy and Spectroscopy in Plant Cell Characterization journal March 2018
Peroxidases Bound to the Growing Lignin Polymer Produce Natural Like Extracellular Lignin in a Cell Culture of Norway Spruce journal October 2016
Polarization Sensitivity in Scattering-Type Scanning Near-Field Optical Microscopy—Towards Nanoellipsometry journal September 2023