U.S. Department of EnergyOffice of Scientific and Technical Information
HSQC spectra of lignin isolated from poplar stems
Abstract
Here we present a curated dataset of two-dimensional heteronuclear single quantum coherence (HSQC) nuclear magnetic resonance (NMR) spectra of lignin isolated from stems of genetically engineered poplar through auxin signaling gene modification. The plants were grown in greenhouse with temperatures between 21 and 23 °C. Plants were harvested and the aboveground stems were cut off an approximately five-inch-long segment from the bottom end of the plant stem, debarked and air-dried for three weeks. The dried stem samples were Wiley milled (mesh size 20), Soxhlet-extracted with toluene/ethanol for 24 h to remove extractives. The extracted biomass was ball-milled in a Retsch PM100 planetary ball mill using a porcelain jar with ceramic balls at 600 rpm for 2 h (in 5 min on and 5 min off cycles to avoid excessive sample heating). 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 freeze-dried to recover the lignin. The dry stem lignin samples were dissolved in deuterated dimethyl sulfoxide (d6) and transferred into a 5 mm tube. 13C–1H HSQC experiments were performed in a Bruker Avance III HD 500 MHz NMR spectrometer operating at a frequency of 125.12more »
- Authors:
-
- Department of Chemical and Biomolecular Engineering, University of Tennessee Knoxville, Knoxville, TN, USA
- Joint Institute for Biological Sciences, Bioscience Division, Oak Ridge National Laboratory, Oak Ridge, TN, 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 Joint Institute for Biological Sciences, Bioscience Division, Oak Ridge National Laboratory, Oak Ridge, TN, USA Center for Bioenergy Innovation, Oak Ridge National Laboratory, Oak Ridge, TN, USA
- Publication Date:
- 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). Biological Systems Science (BSS)
- Subject:
- HSQC, lignin, poplar, stems, CBI
- OSTI Identifier:
- 2447131
- DOI:
- https://doi.org/10.25983/2447131
Citation Formats
Kousika, Rohit, Yunqiao, Pu, Kalluri, Udaya, and Ragauskas, Art. HSQC spectra of lignin isolated from poplar stems. United States: N. p., 2024.
Web. doi:10.25983/2447131.
Kousika, Rohit, Yunqiao, Pu, Kalluri, Udaya, & Ragauskas, Art. HSQC spectra of lignin isolated from poplar stems. United States. doi:https://doi.org/10.25983/2447131
Kousika, Rohit, Yunqiao, Pu, Kalluri, Udaya, and Ragauskas, Art. 2024.
"HSQC spectra of lignin isolated from poplar stems". United States. doi:https://doi.org/10.25983/2447131. https://www.osti.gov/servlets/purl/2447131. Pub date:Fri Sep 20 00:00:00 EDT 2024
@article{osti_2447131,
title = {HSQC spectra of lignin isolated from poplar stems},
author = {Kousika, Rohit and Yunqiao, Pu and Kalluri, Udaya and Ragauskas, Art},
abstractNote = {Here we present a curated dataset of two-dimensional heteronuclear single quantum coherence (HSQC) nuclear magnetic resonance (NMR) spectra of lignin isolated from stems of genetically engineered poplar through auxin signaling gene modification. The plants were grown in greenhouse with temperatures between 21 and 23 °C. Plants were harvested and the aboveground stems were cut off an approximately five-inch-long segment from the bottom end of the plant stem, debarked and air-dried for three weeks. The dried stem samples were Wiley milled (mesh size 20), Soxhlet-extracted with toluene/ethanol for 24 h to remove extractives. The extracted biomass was ball-milled in a Retsch PM100 planetary ball mill using a porcelain jar with ceramic balls at 600 rpm for 2 h (in 5 min on and 5 min off cycles to avoid excessive sample heating). 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 freeze-dried to recover the lignin. The dry stem lignin samples were dissolved in deuterated dimethyl sulfoxide (d6) and transferred into a 5 mm tube. 13C–1H HSQC 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 on a Prodigy platform cryoprobe. The NMR spectra were acquired under the following acquisition conditions: 230 ppm spectral width in F1 (13C) dimension with 256 data points and 12 ppm spectral width in F2 (1H) dimension with 2048 data points, a 90° pulse, a one bond C–H coupling constant of 145 Hz, a 1.0 s pulse delay, and 64 scans. Spectra were processed using the Bruker TopSpin 3.6 software. Additional meta data is embedded in the raw spectra figures.},
doi = {10.25983/2447131},
journal = {},
number = ,
volume = ,
place = {United States},
year = {Fri Sep 20 00:00:00 EDT 2024},
month = {Fri Sep 20 00:00:00 EDT 2024}
}