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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. ISSN 1463-9076

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

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:

Date	Event
2011	Published

Volume:

Vol.13

Number:

No.26

Page Range:

pp. 12213-12224

Identification Number:

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)

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