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双核增强再偶合技术用于高效的氘代蛋白 13C MAS NMR 相关谱学研究。

Double-nucleus enhanced recoupling for efficient 13C MAS NMR correlation spectroscopy of perdeuterated proteins.

机构信息

Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rossle-Str. 10, 13125 Berlin, Germany.

出版信息

J Am Chem Soc. 2009 Dec 2;131(47):17054-5. doi: 10.1021/ja907493p.

Abstract

The use of both proton and deuterium dipolar coupling networks to obtain efficient (13)C magic-angle-spinning NMR correlation spectroscopy is introduced. This new strategy aims to improve the efficiency of (13)C spin diffusion in perdeuterated proteins. The method is called double-nucleus enhanced recoupling (DONER), and it provides significantly improved transfer efficiency for carbon spin diffusion at low proton density. The C(alpha) cross-peak intensity in the DONER experiment is approximately 3 and approximately 5 times stronger than those in conventional radio-frequency-assisted diffusion (RAD) and proton-driven spin diffusion (PDSD) experiments, respectively. Remarkably, the full cross-peak pattern for the aliphatic region of an extensively perdeuterated SH3 protein sample can be obtained using the DONER approach with direct (13)C excitation.

摘要

介绍了一种同时利用质子和氘核偶极耦合网络获得高效(13)C魔角旋转 NMR 相关光谱的方法。该新策略旨在提高氘代蛋白质中(13)C 自旋扩散的效率。该方法称为双核增强再偶联(DONER),它在低质子密度下提供了显著提高的碳自旋扩散的转移效率。在 DONER 实验中,C(alpha)交叉峰强度分别比常规射频辅助扩散(RAD)和质子驱动自旋扩散(PDSD)实验中的强度强约 3 倍和约 5 倍。值得注意的是,使用 DONER 方法直接(13)C 激发可以获得广泛氘代 SH3 蛋白样品的脂肪族区域的全交叉峰图案。

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