Characterization of nonderivatized plant cell walls using high-resolution solution-state NMR spectroscopy

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Abstract

A recently described plant cell wall dissolution system has been modified to use perdeuterated solvents to allow direct in-NMR-tube dissolution and high-resolution solution-state NMR of the whole cell wall without derivatization. Finely ground cell wall material dissolves in a solvent system containing dimethylsulfoxide-d6 and 1-methylimidazole-d6 in a ratio of 4:1 (v/v), keeping wood component structures mainly intact in their near-native state. Two-dimensional NMR experiments, using gradient-HSQC (heteronuclear single quantum coherence) 1 -bond 13C-1H correlation spectroscopy, on nonderivatized cell wall material from a representative gymnosperm Pinus taeda (loblolly pine), an angiosperm Populus tremuloides (quaking aspen), and a herbaceous plant Hibiscus cannabinus (kenaf) demonstrate the efficacy of the system. We describe a method to synthesize 1-methylimidazole-d6 with a high degree of perdeuteration, thus allowing cell wall dissolution and NMR characterization of nonderivatized plant cell wall structures. Copyright © 2008 John Wiley & Sons, Ltd.

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Yelle, D. J., Ralph, J., & Frihart, C. R. (2008). Characterization of nonderivatized plant cell walls using high-resolution solution-state NMR spectroscopy. Magnetic Resonance in Chemistry, 46(6), 508–517. https://doi.org/10.1002/mrc.2201

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