NMR of Fully and Partially ¹³ C-Enriched Biomass Enhances Pendent Group Structural Characterization
Abstract
Traditional solution-state NMR experiments may either fail or yield unsatisfactory results when employing fully-13 Clabeled biomass due to complications arising from 13 C-13 C coupling. Constant-time analogs of HSQC experiments mitigate such issues and deliver enhanced sensitivity. A rarely reported CT-HSQC-TOCSY experiment allows the proton coupling network to deliver much of the same value as the parent experiment on unlabeled or 10-15%-13 C-labeled biomass polymers but with enhanced sensitivity. In the absence of a viable HMBC analog for long-range correlations, a relayed C-C experiment, i.e., via directly bonded 13 C-labeled networks, enables the reliable assignment of coupled carbons, with the added advantage of correlating the more elusive quaternaries. A C-C-FLOPSY experiment takes advantage of fully-13 C-labeled materials for mapping extensive carbon networks in the complex polymer mixtures inherent in biomass. Various pendent groups (tricin units, cis-and trans-p-coumarates, and p-hydroxybenzoates) that adorn lignins, and the cis-and trans-ferulates on arabinoxylan polysaccharides, are exquisitely revealed in spectra from isolated lignins or whole-cell-wall materials from maize, sorghum, and poplar.
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BibTeX
@article{ralph2026fully,
title = {{NMR of Fully and Partially ¹³ C-Enriched Biomass Enhances Pendent Group Structural Characterization}},
author = {John Ralph and Guy Lippens and Marco Tonelli and Charles G Fry and Clemens Anklin and Fachuang Lu and Vitaliy I Timokhin and Rebecca A Smith and Sarah Liu and Sally A Ralph and Wu Lan and Yuki Tobimatsu and Fengxia Yue and Yanding Li and Mirko Bunzel and Mathias Sorieul and Stefan Hill and Shawn D Mansfield and Wout Boerjan and Marc Van Montagu and Jorge Rencoret and José C del Río and Yu Gao and Jenny C Mortimer},
journal = {Analytical Chemistry},
year = {2026},
month = jun,
doi = {10.1021/acs.analchem.5c08043},
url = {https://hal.inrae.fr/hal-05784164v1},
note = {CC BY 4.0},
}
RIS
TY - JOUR
TI - NMR of Fully and Partially ¹³ C-Enriched Biomass Enhances Pendent Group Structural Characterization
AU - John Ralph
AU - Guy Lippens
AU - Marco Tonelli
AU - Charles G Fry
AU - Clemens Anklin
AU - Fachuang Lu
AU - Vitaliy I Timokhin
AU - Rebecca A Smith
AU - Sarah Liu
AU - Sally A Ralph
AU - Wu Lan
AU - Yuki Tobimatsu
AU - Fengxia Yue
AU - Yanding Li
AU - Mirko Bunzel
AU - Mathias Sorieul
AU - Stefan Hill
AU - Shawn D Mansfield
AU - Wout Boerjan
AU - Marc Van Montagu
AU - Jorge Rencoret
AU - José C del Río
AU - Yu Gao
AU - Jenny C Mortimer
PY - 2026
DA - 2026/06/23
JO - Analytical Chemistry
DO - 10.1021/acs.analchem.5c08043
UR - https://hal.inrae.fr/hal-05784164v1
AB - Traditional solution-state NMR experiments may either fail or yield unsatisfactory results when employing fully-13 Clabeled biomass due to complications arising from 13 C-13 C coupling. Constant-time analogs of HSQC experiments mitigate such issues and deliver enhanced sensitivity. A rarely reported CT-HSQC-TOCSY experiment allows the proton coupling network to deliver much of the same value as the parent experiment on unlabeled or 10-15%-13 C-labeled biomass polymers but with enhanced sensitivity. In the absence of a viable HMBC analog for long-range correlations, a relayed C-C experiment, i.e., via directly bonded 13 C-labeled networks, enables the reliable assignment of coupled carbons, with the added advantage of correlating the more elusive quaternaries. A C-C-FLOPSY experiment takes advantage of fully-13 C-labeled materials for mapping extensive carbon networks in the complex polymer mixtures inherent in biomass. Various pendent groups (tricin units, cis-and trans-p-coumarates, and p-hydroxybenzoates) that adorn lignins, and the cis-and trans-ferulates on arabinoxylan polysaccharides, are exquisitely revealed in spectra from isolated lignins or whole-cell-wall materials from maize, sorghum, and poplar.
SN - 0003-2700
SN - 1520-6882
ER -