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Ultra-high resolution 17O solid-state NMR spectroscopy of biomolecules : a comprehensive spectral analysis of monosodium L-glutamate·monohydrate

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Wong, Alan, Howes, Andrew P., Yates, Jonathan R., Watts, A., Anupõld, Tiit, Past, Jaan, Samoson, Ago, Dupree, Ray and Smith, Mark E. (2011) Ultra-high resolution 17O solid-state NMR spectroscopy of biomolecules : a comprehensive spectral analysis of monosodium L-glutamate·monohydrate. Physical Chemistry Chemical Physics, Vol.13 (No.26). pp. 12213-12224. doi:10.1039/c1cp20629j

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Official URL: http://dx.doi.org/10.1039/c1cp20629j

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Abstract

Monosodium L-glutamate monohydrate, a multiple oxygen site (eight) compound, is used to demonstrate that a combination of high-resolution solid-state NMR spectroscopic techniques opens up new possibilities for (17)O as a nuclear probe of biomolecules. Eight oxygen sites have been resolved by double rotation (DOR) and multiple quantum (MQ) NMR experiments, despite the (17)O chemical shifts lying within a narrow shift range of <50 ppm. (17)O DOR NMR not only provides high sensitivity and spectral resolution, but also allows a complete set of the NMR parameters (chemical shift anisotropy and electric-field gradient) to be determined from the DOR spinning-sideband manifold. These (17)O NMR parameters provide an important multi-parameter comparison with the results from the quantum chemical NMR calculations, and enable unambiguous oxygen-site assignment and allow the hydrogen positions to be refined in the crystal lattice. The difference in sensitivity between DOR and MQ NMR experiments of oxygen in bio/organic molecules is also discussed. The data presented here clearly illustrates that a high resolution (17)O solid-state NMR methodology is now available for the study of biomolecules, offering new opportunities for resolving structural information and hence new molecular insights.

Item Type: Journal Article
Subjects: Q Science > QC Physics
Divisions: Administration > Vice Chancellor's Office
Faculty of Science > Physics
Library of Congress Subject Headings (LCSH): Nuclear magnetic resonance spectroscopy, Biomolecules -- Analysis
Journal or Publication Title: Physical Chemistry Chemical Physics
Publisher: Royal Society of Chemistry
ISSN: 1463-9076
Official Date: 2011
Dates:
DateEvent
2011Published
Volume: Vol.13
Number: No.26
Page Range: pp. 12213-12224
DOI: 10.1039/c1cp20629j
Status: Peer Reviewed
Publication Status: Published
Access rights to Published version: Restricted or Subscription Access
Funder: Engineering and Physical Sciences Research Council (EPSRC), Biotechnology and Biological Sciences Research Council (Great Britain) (BBSRC), University of Warwick, Estonian Science Foundation (ESF), Natural Sciences and Engineering Research Council of Canada (NSERC), Leverhulme Trust (LT), Corpus Christi College (University of Cambridge)
Grant number: BB/C000471/1 (BBSRC)

Data sourced from Thomson Reuters' Web of Knowledge

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