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通过同核偶极耦合实现适度的核间选择转移的偏移量差。

Modest Offset Difference Internuclear Selective Transfer via Homonuclear Dipolar Coupling.

机构信息

Department of NMR Based Structural Biology, Max Planck Institute for Biophysical Chemistry, Am Fassberg 11, 37077 Göttingen, Germany.

出版信息

J Phys Chem Lett. 2022 Feb 17;13(6):1540-1546. doi: 10.1021/acs.jpclett.1c03871. Epub 2022 Feb 8.

DOI:10.1021/acs.jpclett.1c03871
PMID:35133845
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC8859849/
Abstract

Homonuclear dipolar recoupling is routinely used for magic-angle spinning NMR-based structure determination. In fully protonated samples, only short proton-proton distances are accessible to broadband recoupling approaches because of high proton density. Selective methods allow detection of longer distances by directing polarization to a subset of spins. Here we introduce the selective pulse sequence MODIST, which recouples spins that have a modest chemical shift offset difference, and demonstrate it to selectively record correlations between amide protons. The sequence was selected for good retention of total signal, leading to up to twice the intensity for proton-proton correlations compared with other selective methods. The sequence is effective across a range of spinning conditions and magnetic fields, here tested at 55.555 and 100 kHz magic-angle spinning and at proton Larmor frequencies from 600 to 1200 MHz. For influenza A M2 in lipid bilayers, cross-peaks characteristic of a helical conformation are observed.

摘要

同核双自旋偶极去偶在魔角旋转 NMR 结构测定中被广泛应用。在完全质子化的样品中,由于质子密度高,宽带偶极去偶方法只能探测到短的质子-质子距离。选择性方法通过将极化定向到自旋子集来检测更长的距离。本文介绍了一种选择性脉冲序列 MODIST,该序列可以偶合化学位移偏移差适中的自旋,并证明其可用于选择性记录酰胺质子之间的相关。该序列的选择是为了保持总信号的良好保留,与其他选择性方法相比,质子-质子相关的强度提高了一倍。该序列在多种旋转条件和磁场下均有效,在此测试了在 55.555 和 100 kHz 魔角旋转以及质子拉莫尔频率为 600 至 1200 MHz 的情况下的效果。在脂质双层中的流感 A M2 中,观察到了特征为螺旋构象的交叉峰。

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