Characterization of nonderivatized plant cell walls using high-resolution solution-state NMR spectroscopy.
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-d(6) and 1-methylimidazole-d(6) 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--(1)H 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-d(6) with a high degree of perdeuteration, thus allowing cell wall dissolution and NMR characterization of nonderivatized plant cell wall structures.
Yelle
Daniel J
DJ
USDA Forest Service, Forest Products Laboratory, Madison, Wisconsin, USA.
Ralph
John
J
Frihart
Charles R
CR
D002458:Cell Fractionation / Q000379:methods*; D002462:Cell Membrane / Q000737:chemistry*; D019906:Nuclear Magnetic Resonance, Biomolecular / Q000379:methods*; D010936:Plant Extracts / Q000032:analysis* / Q000737:chemistry*; D012680:Sensitivity and Specificity; D012997:Solvents / Q000737:chemistry; D013048:Specimen Handling / Q000379:methods*
D010936:Plant Extracts; D012997:Solvents