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Nuclear magnetic resonance (NMR) analysis of entire plant cell walls without isolating their components gained importance over the last decade. Recently, a dissolution method and an NMR analysis of entire plant cell walls were reported, in which finely ball-milled lignocellulosic biomass was dissolved at 100°C in the ionic liquid (IL) 1-butyl-3-methylimidazolium chloride. In the present study, several ILs were examined with or without co-solvent to find milder dissolution conditions to mitigate possible degradation processes. Co-solvents, including  N , N -dimethylacetamide, pyridine, and dimethyl sulfoxide, increased the solubilization efficiency of ILs. For example, ball-milled fir wood was completely dissolved in 1-allyl-3-methylimidazolium chloride ([Amim]Cl) at 30°C in the presence of these co-solvents. The heteronuclear single-quantum coherence NMR spectra of acetylated fir, birch, and bamboo cell walls, which were recovered from [Amim]Cl/pyridine (1:1, w/w) solution, had a high analytical power.

holzforschung

Dissolution and acetylation of ball-milled lignocellulosic biomass in ionic liquids at room temperature: application to nuclear magnetic resonance analysis of cell-wall components