Journal
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
Volume 58, Issue 18, Pages 9882-9892Publisher
AMER CHEMICAL SOC
DOI: 10.1021/jf101258x
Keywords
Milled wood lignin; solid-state NMR; heterogeneity; spin diffusion; spectral editing
Funding
- National Science Foundation [EAR-0843996, CBET-0853950]
- Directorate For Engineering
- Div Of Chem, Bioeng, Env, & Transp Sys [0853950] Funding Source: National Science Foundation
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Advanced solid-state NMR was employed to investigate differences in chemical structure and heterogeneity between milled wood lignin (MWL) and residual enzyme lignin (REL). Wiley and conventional milled woods were also studied. The advanced NMR techniques included C-13 quantitative direct polarization, various spectral-editing techniques, and two-dimensional H-1-C-13 heteronuclear correlation NMR with H-1 spin diffusion. The C-13 chemical shift regions between 110 and 160 ppm of two lignins were quite similar to those of two milled woods. REL contained much more residual carbohydrates than MWL, showing that MWL extraction more successfully separated lignin from cellulose and hemicelluloses than REL extraction; REL was also of higher COO, aromatic C-C, and condensed aromatics but of lower aromatic C-H. At a spin diffusion time of 0.55 ms, the magnetization was equilibrated through the whole structure of MWL lignin, but not through that of REL, indicating that REL is more heterogeneous than MWL.
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