A Time-Saving Strategy for MAS NMR Spectroscopy by Combining Nonuniform Sampling and Paramagnetic Relaxation Assisted Condensed Data Collection

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• 作者：Shangjin Sun ; Si Yan ; Changmiao Guo ; Mingyue Li ; Jeffrey C. Hoch ; John C. Williams ; Tatyana Polenova
• 刊名：The Journal of Physical Chemistry B
• 出版年：2012
• 出版时间：November 26, 2012
• 年：2012
• 卷：116
• 期：46
• 页码：13585-13596
• 全文大小：615K
• 年卷期：v.116,no.46(November 26, 2012)
• ISSN：1520-5207

文摘

We present a time-saving strategy for acquiring 3D magic angle spinning NMR spectra for chemical shift assignments in proteins and protein assemblies in the solid state. By simultaneous application of nonuniform sampling (NUS) and paramagnetic-relaxation-assisted condensed data collection (PACC), we can attain 16-fold time reduction in the 3D experiments without sacrificing the signal-to-noise ratio or the resolution. We demonstrate that with appropriate concentration of paramagnetic dopant introduced into the sample the overwhelming majority of chemical shifts are not perturbed, with the exception of a limited number of shifts corresponding to residues located at the surface of the protein, which exhibit small perturbations. This approach enables multidimensional MAS spectroscopy in samples of intrinsically low sensitivity and/or high spectral congestion where traditional experiments fail, and is especially beneficial for structural and dynamics studies of large proteins and protein assemblies.