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Xue, K.* ; Sarkar, R. ; Tosner, Z.* ; Reif, B.

Field and magic angle spinning frequency dependence of proton resonances in rotating solids.

Prog. Nucl. Magn. Reson. Spectrosc. 130-131, 45-59 (2022)
Postprint DOI PMC
Open Access Green
Proton detection in solid state NMR is continuously developing and allows one to gain new insights in structural biology. Overall, this progress is a result of the synergy between hardware development, new NMR methodology and new isotope labeling strategies, to name a few factors. Even though current developments are rapid, it is worthwhile to summarize what can currently be achieved employing proton detection in biological solids. We illustrate this by analysing the signal-to-noise ratio (SNR) for spectra obtained for a microcrystalline α-spectrin SH3 domain protein sample by (i) employing different degrees of chemical dilution to replace protons by incorporating deuterons in different sites, by (ii) variation of the magic angle spinning (MAS) frequencies between 20 and 110 kHz, and by (iii) variation of the static magnetic field B0. The experimental SNR values are validated with numerical simulations employing up to 9 proton spins. Although in reality a protein would contain far more than 9 protons, in a deuterated environment this is a sufficient number to achieve satisfactory simulations consistent with the experimental data. The key results of this analysis are (i) with current hardware, deuteration is still necessary to record spectra of optimum quality; (ii) 13CH3 isotopomers for methyl groups yield the best SNR when MAS frequencies above 100 kHz are available; and (iii) sensitivity increases with a factor beyond B0 3/2 with the static magnetic field due to a transition of proton-proton dipolar interactions from a strong to a weak coupling limit.
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Publication type Article: Journal article
Document type Review
Corresponding Author
Keywords Biological Solids ; Magic Angle Spinning ; Proton Detection ; Solid State Nmr
ISSN (print) / ISBN 0079-6565
e-ISSN 1873-3301
Journal Progress in Nuclear Magnetic Resonance Spectroscopy
Quellenangaben Volume: 130-131, Issue: , Pages: 45-59 Article Number: , Supplement: ,
Publisher Elsevier
Publishing Place Oxford
Non-patent literature Publications
Reviewing status Peer reviewed
Institute(s) Institute of Structural Biology (STB)
Grants Grantová Agentura České Republiky
Ministerstvo Školství, Mládeže a Tělovýchovy
Deutsche Forschungsgemeinschaft
Helmholtz-Gemeinschaft
Center for Integrated Protein Science Munich