Carbon-13 NMR spectra of lignin isolated from field grown transgenic poplar

Pu, Yunqiao; Bryant, Nathan; Liu, Chang-Jun; Ragauskas, Arthur

doi:10.25983/2440812

Title: Carbon-13 NMR spectra of lignin isolated from field grown transgenic poplar

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Abstract

Here we present a curated dataset of a series of 13C nuclear magnetic resonance (NMR) spectra of lignin isolated from transgenic monolignol 4-O-methyltransferase (MOMT4) engineered poplar. The transgenic poplar was collected from a 3-year field trial experiment. The poplar was Soxhlet-extracted with toluene/ethanol and the extractives-free poplar was then ball-milled in a Retsch PM100 planetary ball mill using a porcelain jar with ceramic balls at 600 rpm for 2 h. The ball-milled materials were then subjected to enzymatic hydrolysis for 48 h followed by centrifugation and washing with deionized water. The solid residue was extracted twice with 96:4 (v/v) 1,4-dioxane/water mixture at room temperature overnight. The extracts were combined, rotary evaporated, and freeze-dried to recover the lignin. The dry lignin samples were dissolved in deuterated dimethyl sulfoxide for NMR characterization. 13C experiments were performed in a Bruker Avance III HD 500 MHz NMR spectrometer operating at a frequency of 125.12 MHz for the 13C nucleus using a standard Bruker pulse sequence (zgpg) on a Prodigy platform cryoprobe. The NMR spectra were acquired under the following conditions: spectra width 229 ppm, 64k data points, 1s pulse delay, and 6k scans. All the data was processed using the Bruker’s TopSpin 3.6 software.more »« less

Authors:

Pu, Yunqiao; Bryant, Nathan; Liu, Chang-Jun; Ragauskas, Arthur

Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States). Center for Bioenergy Innovation (CBI)
University of Tennessee, Knoxville. Center for Bioenergy Innovation (CBI)
Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States). Center for Bioenergy Innovation (CBI) Biology Department, Brookhaven National Laboratory, Upton, New York, USA
Center for Bioenergy Innovation, Oak Ridge National Laboratory, Oak Ridge, TN, USA Department of Chemical and Biomolecular Engineering, University of Tennessee Knoxville, Knoxville, TN, USA

Publication Date:: Thu Sep 12 00:00:00 EDT 2024

DOE Contract Number:: AC05-00OR22725

Research Org.:: Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)

Sponsoring Org.:: USDOE Office of Science (SC), Biological and Environmental Research (BER).

Subject:: 13C NMR, lignin, poplar, field trial, MOMT4, CBI

OSTI Identifier:: 2440812

DOI:: https://doi.org/10.25983/2440812

Citation Formats


                    Pu, Yunqiao, Bryant, Nathan, Liu, Chang-Jun, and Ragauskas, Arthur. Carbon-13 NMR spectra of lignin isolated from field grown transgenic poplar.  United States: N. p., 2024. 
        Web.  doi:10.25983/2440812.

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                    Pu, Yunqiao, Bryant, Nathan, Liu, Chang-Jun, & Ragauskas, Arthur. Carbon-13 NMR spectra of lignin isolated from field grown transgenic poplar.  United States.  doi:https://doi.org/10.25983/2440812

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                    Pu, Yunqiao, Bryant, Nathan, Liu, Chang-Jun, and Ragauskas, Arthur. 2024.  
"Carbon-13 NMR spectra of lignin isolated from field grown transgenic poplar".  United States.  doi:https://doi.org/10.25983/2440812.  https://www.osti.gov/servlets/purl/2440812. Pub date:Thu Sep 12 00:00:00 EDT 2024

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@article{osti_2440812,

  title        = {Carbon-13 NMR spectra of lignin isolated from field grown transgenic poplar},

  author       = {Pu, Yunqiao and Bryant, Nathan and Liu, Chang-Jun and Ragauskas, Arthur},

  abstractNote = {Here we present a curated dataset of a series of 13C nuclear magnetic resonance (NMR) spectra of lignin isolated from transgenic monolignol 4-O-methyltransferase (MOMT4) engineered poplar. The transgenic poplar was collected from a 3-year field trial experiment. The poplar was Soxhlet-extracted with toluene/ethanol and the extractives-free poplar was then ball-milled in a Retsch PM100 planetary ball mill using a porcelain jar with ceramic balls at 600 rpm for 2 h. The ball-milled materials were then subjected to enzymatic hydrolysis for 48 h followed by centrifugation and washing with deionized water. The solid residue was extracted twice with 96:4 (v/v) 1,4-dioxane/water mixture at room temperature overnight. The extracts were combined, rotary evaporated, and freeze-dried to recover the lignin. The dry lignin samples were dissolved in deuterated dimethyl sulfoxide for NMR characterization. 13C experiments were performed in a Bruker Avance III HD 500 MHz NMR spectrometer operating at a frequency of 125.12 MHz for the 13C nucleus using a standard Bruker pulse sequence (zgpg) on a Prodigy platform cryoprobe. The NMR spectra were acquired under the following conditions: spectra width 229 ppm, 64k data points, 1s pulse delay, and 6k scans. All the data was processed using the Bruker’s TopSpin 3.6 software. Additional meta data is embedded in the raw spectra files.},

  doi          = {10.25983/2440812},

  journal      = {},

  number       = ,

  volume       = ,

  place        = {United States},

  year         = {Thu Sep 12 00:00:00 EDT 2024},

  month        = {Thu Sep 12 00:00:00 EDT 2024}

}

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DOI: https://doi.org/10.25983/2440812

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