[superscript 2]H-DNP-enhanced [superscript 2]H-[superscript 13]C solid-state NMR correlation spectroscopy
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2HDNP_100422_final_RGG.pdf
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Author(s) • • •
Maly, Thorsten
Andreas, Loren
Griffin, Robert Guy
Smith, Albert A.
Date Issued
May 2010
Journal
Physical Chemistry Chemical Physics
Publisher
Royal Society of Chemistry, The
Citation
Maly, Thorsten et al. “2H-DNP-enhanced 2H–13C Solid-state NMR Correlation Spectroscopy.” Physical Chemistry Chemical Physics 12.22 (2010): 5872.
Version
Author's final manuscript
Abstract
Perdeuteration of biological macromolecules for magic angle spinning solid-state NMR spectroscopy can yield high-resolution [superscript 2]H–[superscript 13]C correlation spectra and the method is therefore of great interest for the structural biology community. Here we demonstrate that the combination of sample deuteration and dynamic nuclear polarization yields resolved [superscript 2]H–[superscript 13]C correlation spectra with a signal enhancement of ε ≥ 700 compared to a spectrum recorded with microwaves off and otherwise identical conditions. To our knowledge, this is the first time that [superscript 2]2H-DNP has been employed to enhance MAS-NMR spectra of a biologically relevant system. The DNP process is studied using several polarizing agents and the technique is applied to obtain [superscript 2]H–[superscript 13]C correlation spectra of U-[[superscript 2]H, [superscript 13]C] proline.
MIT Department
Massachusetts Institute of Technology. Department of Chemistry
Francis Bitter Magnet Laboratory (Massachusetts Institute of Technology)
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Creative Commons Attribution-Noncommercial-Share Alike 3.0
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DOI of Published Version
https://doi.org/10.1039/c003705b