Accelerating 15N and 13C R1 and R1ρ relaxation measurements by multiple pathway solid-state NMR experiments

被引:4
作者
Tognetti, Jacqueline [1 ,2 ]
Franks, W. Trent [1 ,2 ]
Gallo, Angelo [2 ]
Lewandowski, Jozef R. [2 ]
机构
[1] Univ Warwick, Dept Phys, Coventry CV4 7AL, W Midlands, England
[2] Univ Warwick, Dept Chem, Coventry CV4 7AL, W Midlands, England
基金
英国生物技术与生命科学研究理事会; 欧洲研究理事会; 英国工程与自然科学研究理事会;
关键词
Solid-state NMR; Magic angle spinning; NMR relaxation; Staggered acquisition; DRIVEN SPIN-DIFFUSION; SIMULTANEOUS ACQUISITION; BACKBONE DYNAMICS; SENSITIVITY ENHANCEMENT; PARAMAGNETIC RELAXATION; PROTEIN; SPECTROSCOPY; ASSIGNMENT; SYSTEMS; H-1;
D O I
10.1016/j.jmr.2021.107049
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
Magic angle spinning (MAS) Solid-state NMR is a powerful technique to probe dynamics of biological systems at atomic resolution. R-1 and R-1 rho relaxation measurements can provide detailed insight on amplitudes and time scales of motions, especially when information from several different site-specific types of probes is combined. However, such experiments are time-consuming to perform. Shortening the time necessary to record relaxation data for different nuclei will greatly enhance practicality of such approaches. Here, we present staggered acquisition experiments to acquire multiple relaxation experiments from a single excitation to reduce the overall experimental time. Our strategy enables one to collect N-15 and C-13 relaxation data in a single experiment in a fraction of the time necessary for two separate experiments, with the same signal to noise ratio. (C) 2021 The Authors. Published by Elsevier Inc.
引用
收藏
页数:11
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共 48 条
[11]   Dual Acquisition Magic-Angle Spinning Solid-State NMR-Spectroscopy: Simultaneous Acquisition of Multidimensional Spectra of Biomacromolecules [J].
Gopinath, T. ;
Veglia, Gianluigi .
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION, 2012, 51 (11) :2731-2735
[12]   Distance information from proton-driven spin diffusion under MAS [J].
Grommek, Andreas ;
Meier, Beat H. ;
Ernst, Matthias .
CHEMICAL PHYSICS LETTERS, 2006, 427 (4-6) :404-409
[13]   THE MEASUREMENT OF HETERONUCLEAR TRANSVERSE RELAXATION-TIMES IN AX3 SPIN SYSTEMS VIA POLARIZATION-TRANSFER TECHNIQUES [J].
KAY, LE ;
BULL, TE ;
NICHOLSON, LK ;
GRIESINGER, C ;
SCHWALBE, H ;
BAX, A ;
TORCHIA, DA .
JOURNAL OF MAGNETIC RESONANCE, 1992, 100 (03) :538-558
[14]   15N spin diffusion rate in solid-state NMR of totally enriched proteins:: The magic angle spinning frequency effect [J].
Krushelnitsky, Alexey ;
Braeuniger, Thomas ;
Reichert, Detlef .
JOURNAL OF MAGNETIC RESONANCE, 2006, 182 (02) :339-342
[15]   The nuclear magnetic resonance relaxation data analysis in solids: General R1/R1ρ equations and the model-free approach [J].
Kurbanov, Rauf ;
Zinkevich, Tatjana ;
Krushelnitsky, Alexey .
JOURNAL OF CHEMICAL PHYSICS, 2011, 135 (18)
[16]   Relaxation-Based Magic-Angle Spinning NMR Approaches for Studying Protein Dynamics [J].
Lamley, Jonathan M. ;
Lewandowski, Jozef R. .
EMAGRES, 2016, 5 (03) :1423-1433
[17]   Intermolecular Interactions and Protein Dynamics by Solid-State NMR Spectroscopy [J].
Lamley, Jonathan M. ;
Oester, Carl ;
Stevens, Rebecca A. ;
Lewandowski, Jozef R. .
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION, 2015, 54 (51) :15374-15378
[18]   Unraveling the complexity of protein backbone dynamics with combined 13C and 15N solid-state NMR relaxation measurements [J].
Lamley, Jonathan M. ;
Lougher, Matthew J. ;
Sass, Hans Juergen ;
Rogowski, Marco ;
Grzesiek, Stephan ;
Lewandowski, Jozef R. .
PHYSICAL CHEMISTRY CHEMICAL PHYSICS, 2015, 17 (34) :21997-22008
[19]   Solid-State NMR of a Protein in a Precipitated Complex with a FullLength Antibody [J].
Lamley, Jonathan M. ;
Iuga, Dinu ;
Oester, Carl ;
Sass, Hans-Juergen ;
Rogowski, Marco ;
Oss, Andres ;
Past, Jaan ;
Reinhold, Andres ;
Grzesiek, Stephan ;
Samoson, Ago ;
Lewandowski, Jozef R. .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2014, 136 (48) :16800-16806
[20]   Simultaneous acquisition of homonuclear and heteronuclear long-distance contacts with time-shared third spin assisted recoupling [J].
Lamley, Jonathan M. ;
Lewandowski, Jozef R. .
JOURNAL OF MAGNETIC RESONANCE, 2012, 218 :30-34