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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 13 C-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.
Keywords
NMR,
HSQC,
1 methylimidazole-d6,
dimethylsulfoxide-d6,
Pinus taeda,
Populus tremuloides,
Hibiscus cannabinus,
whole cell wall dissolution,
lignin,
polysaccharides,
chemical reactions,
polysaccharides,
aspen,
ultrastructure,
kenaf,
loblolly pine,
plant cell walls,
wood chemistry,
cellulose,
nuclear magnetic resonance spectroscopy,
acetates,
hemicellulose
Citation
Yelle, Daniel J.; Ralph, John; Frihart, Charles R. 2008. Characterization of nonderivatized plant cell walls using high-resolution solution-state NMR spectroscopy. Magnetic resonance in chemistry. Vol. 46 (2008): pages 508-517.
