New Limits for Solid-State 17O NMR Spectroscopy:  Complete Resolution of Multiple Oxygen Sites in a Simple Biomolecule

A solid-state 17O NMR 1H-decoupled double angle rotation (DOR) study of monosodium l-glutamate monohydrate (l-MSG) is reported. It is shown that all eight inequivalent sites can be resolved with DOR line widths (∼65 Hz) ∼120 times narrower than those in the MAS spectrum. The lines are tentatively as...

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Veröffentlicht in:Journal of the American Chemical Society 2006-06, Vol.128 (24), p.7744-7745
Hauptverfasser: Wong, Alan, Howes, Andy P, Pike, Kevin J, Lemaître, Vincent, Watts, Anthony, Anupõld, Tiit, Past, Jaan, Samoson, Ago, Dupree, Ray, Smith, Mark E
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Sprache:eng
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Zusammenfassung:A solid-state 17O NMR 1H-decoupled double angle rotation (DOR) study of monosodium l-glutamate monohydrate (l-MSG) is reported. It is shown that all eight inequivalent sites can be resolved with DOR line widths (∼65 Hz) ∼120 times narrower than those in the MAS spectrum. The lines are tentatively assigned on the basis of their behavior under proton decoupling and the isotropic chemical shift and the quadrupole interaction parameter for each extracted by a combination of DOR and 3Q MAS at variable magnetic fields. With a shift range of ∼45 ppm for these similar oxygen sites and spectral resolution under DOR comparable to that for spin-1/2 nuclei, solid-state 17O NMR should have tremendous potential in the study of biomolecules.
ISSN:0002-7863
1520-5126
DOI:10.1021/ja062031l