Homonuclear decoupling for enhancing resolution and sensitivity in NOE and RDC measurements of peptides and proteins.
Homonuclear decoupling for enhancing resolution and sensitivity in NOE and RDC measurements of peptides and proteins.
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DOI：
10.1016/j.jmr.2013.11.006
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发表时间：
2014-04
影响因子：
2.2
通讯作者：
Bax, Ad
中科院分区：
文献类型：
--
作者：
Ying, Jinfa;Roche, Julien;Bax, Ad
关键词：
应用频带选择性homopolymers（BASH）1H去耦脉冲在收购过程中的1H自由感应衰减被证明是一个有效的程序，用于去除标量和残余偶极耦合酰胺和脂肪族质子之间。BASH去偶可应用于二维核磁共振实验的两个维度，特别适用于提高肽和蛋白质NOESY光谱的HN-Hα区域的光谱分辨率，这些区域包含有关骨架扭转角的重要信息。然后，该方法还防止零量子和HNz-Hαz项的产生，从而促进残基内相互作用的分析。应用于本质无序蛋白α-突触核蛋白的六肽片段的NOESY谱，突出了线性肽中存在的相当大的扩散各向异性。去除弱对齐蛋白质中HN和脂肪族质子之间的残留偶极偶联增加了光谱的1H-15 N HSQC区域的分辨率，并允许测量相对强对齐的样品中的RDC。该方法被证明用于测量质子化的15 N/13 C富集的泛素中的RDC，在Pf 1中对齐，从而改善了泛素结构的拟合。
Application of band-selective homonuclear (BASH) 1H decoupling pulses during acquisition of the 1H free induction decay is shown to be an efficient procedure for removal of scalar and residual dipolar couplings between amide and aliphatic protons. BASH decoupling can be applied in both dimensions of a homonuclear 2D NMR experiment and is particularly useful for enhancing spectral resolution in the HN-Hα region of NOESY spectra of peptides and proteins, which contain important information on the backbone torsion angles. The method then also prevents generation of zero quantum and HNz-Hαz terms, thereby facilitating analysis of intraresidue interactions. Application to the NOESY spectrum of a hexapeptide fragment of the intrinsically disordered protein α-synuclein highlights the considerable diffusion anisotropy present in linear peptides. Removal of residual dipolar couplings between HN and aliphatic protons in weakly aligned proteins increases resolution in the 1H-15N HSQC region of the spectrum and allows measurement of RDCs in samples that are relatively strongly aligned. The approach is demonstrated for measurement of RDCs in protonated 15N/13C-enriched ubiquitin, aligned in Pf1, yielding improved fitting to the ubiquitin structure.
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影响因子：
2.2
作者：
Ottiger, M;Delaglio, F;Bax, A
通讯作者：
Bax, A
影响因子：
16.6
作者：
Meyer, N. Helge;Zangger, Klaus
通讯作者：
Zangger, Klaus
影响因子：
2.7
作者：
BAX A;IKURA M
通讯作者：
IKURA M
影响因子：
2.2
作者：
MONTELIONE, GT;WAGNER, G
通讯作者：
WAGNER, G
DOI：
10.1006/jmrb.1996.0138
发表时间：
1996-09-01
期刊：
JOURNAL OF MAGNETIC RESONANCE SERIES B
影响因子：
--
作者：
Tolman, JR;Prestegard, JH
通讯作者：
Prestegard, JH