碳检测氘固态核磁共振旋转框架弛豫测量魔角旋转下的蛋白质甲基基团

IF 1.8 3区 化学 Q4 CHEMISTRY, PHYSICAL
Liliya Vugmeyster , Dmitry Ostrovsky , Riqiang Fu
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引用次数: 0

摘要

氘旋转框架固态核磁共振弛豫测量(2H R1ρ)是分子动力学定量研究的重要工具。我们展示了如何将 10-40 kHz 魔角旋转速率下的 2H 至 13C 交叉极化 (CP) 方法与 2H R1ρ 块相结合,从而将氘旋转框架弛豫研究扩展到生物大分子中的甲基。这种扩展允许对 13C 核进行检测,从而实现特定位点的分辨率。我们使用序列为 GGKGMGFGL 的九个残基低复杂性肽进行了测量演示,其中在蛋氨酸残基上放置了单个选择性 -13CD3 标签。我们将碳检测测量结果与氘直接检测结果进行了比较,从而对实验方法进行了微调。特别是,我们展示了绝热呼吸 CP 方案和 2H 与 13C 通道双绝热扫描如何与 2H R1ρ 松弛率测量相结合。除了共振条件之外,我们还研究了非共振 2H R1ρ 测量,因为它们扩大了有效自旋锁定场的范围。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

Carbon-detected deuterium solid-state NMR rotating frame relaxation measurements for protein methyl groups under magic angle spinning

Carbon-detected deuterium solid-state NMR rotating frame relaxation measurements for protein methyl groups under magic angle spinning

Deuterium rotating frame solid-state NMR relaxation measurements (2H R1ρ) are important tools in quantitative studies of molecular dynamics. We demonstrate how 2H to 13C cross-polarization (CP) approaches under 10–40 kHz magic angle spinning rates can be combined with the 2H R1ρ blocks to allow for extension of deuterium rotating frame relaxation studies to methyl groups in biomolecules. This extension permits detection on the 13C nuclei and, hence, for the achievement of site-specific resolution. The measurements are demonstrated using a nine-residue low complexity peptide with the sequence GGKGMGFGL, in which a single selective −13CD3 label is placed at the methionine residue. Carbon-detected measurements are compared with the deuterium direct-detection results, which allows for fine-tuning of experimental approaches. In particular, we show how the adiabatic respiration CP scheme and the double adiabatic sweep on the 2H and 13C channels can be combined with the 2H R1ρ relaxation rates measurement. Off-resonance 2H R1ρ measurements are investigated in addition to the on-resonance condition, as they extent the range of effective spin-locking field.

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来源期刊
CiteScore
5.30
自引率
9.40%
发文量
42
审稿时长
72 days
期刊介绍: The journal Solid State Nuclear Magnetic Resonance publishes original manuscripts of high scientific quality dealing with all experimental and theoretical aspects of solid state NMR. This includes advances in instrumentation, development of new experimental techniques and methodology, new theoretical insights, new data processing and simulation methods, and original applications of established or novel methods to scientific problems.
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