Ultra-High Resolution O-17 Solid-State Nmr Spectroscopy Of Biomolecules: A Comprehensive Spectral Analysis Of Monosodium L-Glutamate Center Dot Monohydrate
PHYSICAL CHEMISTRY CHEMICAL PHYSICS(2011)
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 O-17 as a nuclear probe of biomolecules. Eight oxygen sites have been resolved by double rotation (DOR) and multiple quantum (MQ) NMR experiments, despite the O-17 chemical shifts lying within a narrow shift range of <50 ppm. O-17 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 O-17 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 O-17 solid-state NMR methodology is now available for the study of biomolecules, offering new opportunities for resolving structural information and hence new molecular insights.
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Key words
solid state nmr,high resolution,glutamate
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