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基于自旋回波的固态MAS NMR同核化学位移相关谱中的对角线峰抑制

Spin-echo based diagonal peak suppression in solid-state MAS NMR homonuclear chemical shift correlation spectra.

作者信息

Wang Kaiyu, Zhang Zhiyong, Ding Xiaoyan, Tian Fang, Huang Yuqing, Chen Zhong, Fu Riqiang

机构信息

National High Magnetic Field Lab, 1800 East Paul Dirac Drive, Tallahassee, FL 32310, USA; Department of Electronic Science, Fujian Provincial Key Laboratory of Plasma and Magnetic Resonance, Xiamen University, Xiamen, Fujian 361005, China.

Department of Chemical Physics, Weizman Institute of Science, Rehovot 76100, Israel.

出版信息

J Magn Reson. 2018 Feb;287:91-98. doi: 10.1016/j.jmr.2017.12.019. Epub 2017 Dec 28.

DOI:10.1016/j.jmr.2017.12.019
PMID:29324246
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC6919318/
Abstract

The feasibility of using the spin-echo based diagonal peak suppression method in solid-state MAS NMR homonuclear chemical shift correlation experiments is demonstrated. A complete phase cycling is designed in such a way that in the indirect dimension only the spin diffused signals are evolved, while all signals not involved in polarization transfer are refocused for cancellation. A data processing procedure is further introduced to reconstruct this acquired spectrum into a conventional two-dimensional homonuclear chemical shift correlation spectrum. A uniformly C, N labeled Fmoc-valine sample and the transmembrane domain of a human protein, LR11 (sorLA), in native Escherichia coli membranes have been used to illustrate the capability of the proposed method in comparison with standard C-C chemical shift correlation experiments.

摘要

证明了在固态MAS NMR同核化学位移相关实验中使用基于自旋回波的对角峰抑制方法的可行性。设计了一种完整的相位循环,使得在间接维度中只有自旋扩散信号得以演化,而所有不参与极化转移的信号都被重新聚焦以进行消除。进一步引入了一种数据处理程序,将采集到的谱重建为传统的二维同核化学位移相关谱。使用了一个均匀C、N标记的Fmoc-缬氨酸样品以及天然大肠杆菌膜中的人类蛋白质LR11(sorLA)的跨膜结构域,以说明所提出的方法与标准C-C化学位移相关实验相比的能力。

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本文引用的文献

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J Phys Chem A. 2015 Jan 22;119(3):482-7. doi: 10.1021/jp512511h. Epub 2015 Jan 12.
2
Spectrally edited 2D 13C-13C NMR spectra without diagonal ridge for characterizing 13C-enriched low-temperature carbon materials.无对角峰的谱编辑二维 13C-13C NMR 谱用于表征 13C 富集的低温碳材料。
J Magn Reson. 2013 Sep;234:112-24. doi: 10.1016/j.jmr.2013.06.006. Epub 2013 Jun 22.
3
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J Magn Reson. 2013 Jul;232:1-6. doi: 10.1016/j.jmr.2013.04.005. Epub 2013 Apr 22.
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Spatially encoded ultrafast high-resolution 2D homonuclear correlation spectroscopy in inhomogeneous fields.非均匀场中空间编码的超快高分辨率二维同核相关波谱学。
J Magn Reson. 2013 Feb;227:39-45. doi: 10.1016/j.jmr.2012.11.020. Epub 2012 Nov 29.
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