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使用绝热脉冲的快速MAS全键相关光谱学

Fast-MAS total through-bond correlation spectroscopy using adiabatic pulses.

作者信息

Hardy Edme H, Detken Andreas, Meier Beat H

机构信息

Physical Chemistry, ETH Hoenggerberg, CH-8093 Zurich, Switzerland.

出版信息

J Magn Reson. 2003 Dec;165(2):208-18. doi: 10.1016/j.jmr.2003.08.003.

DOI:10.1016/j.jmr.2003.08.003
PMID:14643702
Abstract

Pulse sequences consisting of adiabatic pulses for total through-bond correlation spectroscopy (TOBSY) under magic-angle spinning (MAS) are introduced. Above a certain threshold, the polarization transfer achieved with these sequences is largely insensitive to the amplitude and homogeneity of the radiofrequency field employed. An experimental transfer efficiency of up to 76% was achieved in a two-spin system using the sequence WiW9(24)(1) at a MAS frequency of 26.67 kHz. Applications to resonance assignments in the dipeptide L-Val-L-Phe and in the cyclic decapeptide antamanide are demonstrated.

摘要

介绍了在魔角旋转(MAS)下用于全键相关光谱(TOBSY)的由绝热脉冲组成的脉冲序列。高于某个阈值时,用这些序列实现的极化转移在很大程度上对所采用射频场的幅度和均匀性不敏感。在一个双自旋系统中,使用序列WiW9(24)(1),在26.67 kHz的MAS频率下,实现了高达76%的实验转移效率。展示了其在二肽L-缬氨酸-L-苯丙氨酸和环十肽蚂蚁毒素的共振归属中的应用。

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