Elucidating Structural Characteristics of Biomass using Solution-State 2 D NMR with a Mixture of Deuterated Dimethylsulfoxide and Hexamethylphosphoramide

Chang Geun Yoo, Yunqiao Pu, Mi Li, Arthur J. Ragauskas

Research output: Contribution to journalArticlepeer-review

63 Scopus citations

Abstract

Recent developments of NMR methods for characterization of lignocellulosic biomass allow improved understanding of plant cell-wall structures with minimal deconstruction and modification of biomass. This study introduces a new NMR solvent system composed of dimethylsulfoxide (DMSO-d6) and hexamethylphosphoramide (HMPA-d18). HMPA as a co-solvent enhanced swelling and mobility of the biomass samples; thereby it allowed enhancing signals of NMR spectra. The structural information of biomass was successfully analyzed by the proposed NMR solvent system (DMSO-d6/HMPA-d18; 4:1, v/v) with different biomass. The proposed bi-solvent system does not require derivatization or isolation of biomass, facilitating a facile sample preparation and involving with no signals overlapping with biomass peaks. It also allows analyzing biomass with a room-temperature NMR probe instead of cryo-probes, which are traditionally used for enhancing signal intensities. Open structures: NMR analysis is a powerful characterization method for understanding biomass structures. Here, we introduce a novel solvent system composed of dimethylsulfoxide (DMSO-d6) and hexamethylphosphoramide (HMPA-d18) for effective cell-wall NMR analysis by improving dissolution/swelling of biomass.

Original languageEnglish
Pages (from-to)1090-1095
Number of pages6
JournalChemSusChem
Volume9
Issue number10
DOIs
StatePublished - May 23 2016

Funding

This manuscript has been authored by UT-Battelle, LLC under Contract No. DE-AC05-00OR22725 with the U.S. Department of Energy. This study was supported and performed as part of the BioEnergy Science Center (BESC). The BioEnergy Science Center is a U.S. Department of Energy Bioenergy Research Center supported by the Office of Biological and Environmental Research in the DOE Office of Science.

Keywords

  • NMR spectroscopy
  • biomass
  • characterization
  • hexamethylphosphoramide
  • whole cell wall

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