High-resolution proton-detected NMR of proteins at very fast MAS

Journal of Magnetic Resonance
Loren B AndreasGuido Pintacuda

Abstract

When combined with high-frequency (currently ∼60 kHz) magic-angle spinning (MAS), proton detection boosts sensitivity and increases coherence lifetimes, resulting in narrow ((1))H lines. Herein, we review methods for efficient proton detected techniques and applications in highly deuterated proteins, with an emphasis on 100% selected ((1))H site concentration for the purpose of sensitivity. We discuss the factors affecting resolution and sensitivity that have resulted in higher and higher frequency MAS. Next we describe the various methods that have been used for backbone and side-chain assignment with proton detection, highlighting the efficient use of scalar-based ((13))C-((13))C transfers. Additionally, we show new spectra making use of these schemes for side-chain assignment of methyl ((13))C-((1))H resonances. The rapid acquisition of resolved 2D spectra with proton detection allows efficient measurement of relaxation parameters used as a measure of dynamic processes. Under rapid MAS, relaxation times can be measured in a site-specific manner in medium-sized proteins, enabling the investigation of molecular motions at high resolution. Additionally, we discuss methods for measurement of structural parameters, including meas...Continue Reading

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Citations

Jan 24, 2016·The Journal of Chemical Physics·Rongchun Zhang, Ayyalusamy Ramamoorthy
Oct 17, 2015·The Journal of Chemical Physics·Rongchun ZhangAyyalusamy Ramamoorthy
Jun 17, 2015·Journal of Biomolecular NMR·Loren B AndreasGuido Pintacuda
Jul 12, 2016·Solid State Nuclear Magnetic Resonance·Yusuke Nishiyama
Aug 5, 2016·Proceedings of the National Academy of Sciences of the United States of America·Loren B AndreasGuido Pintacuda
Feb 24, 2017·Journal of Biomolecular NMR·Abhishek MandalPatrick C A van der Wel
Nov 3, 2015·Journal of Magnetic Resonance·Manoj Kumar PandeyYusuke Nishiyama
Apr 22, 2016·Angewandte Chemie·Hugh R W DannattGuido Pintacuda
Jul 21, 2017·Journal of the American Chemical Society·Daniela LalliGuido Pintacuda
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Jul 6, 2018·Chemical Communications : Chem Comm·Alexander MarchankaTeresa Carlomagno
Aug 10, 2017·Angewandte Chemie·Martins OtikovsKristaps Jaudzems
Nov 20, 2018·Chemphyschem : a European Journal of Chemical Physics and Physical Chemistry·Eszter E NajbauerLoren B Andreas
Nov 22, 2018·Chemistry : a European Journal·Linda CerofoliniClaudio Luchinat
Aug 10, 2017·Chemphyschem : a European Journal of Chemical Physics and Physical Chemistry·Hugo FragaPaul Schanda
Nov 7, 2019·Angewandte Chemie·Brendan M DugganJames J La Clair
Mar 4, 2020·Journal of Biomolecular NMR·Xue KangTuo Wang
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