Longitudinal Relaxation Optimization Enhances H-1-Detected HSQC in Solid-State NMR Spectroscopy on Challenging Biological Systems
Longitudinal Relaxation Optimization Enhances H-1-Detected HSQC in Solid-State NMR Spectroscopy on Challenging Biological Systems
复制标题
纵向弛豫优化增强了具有挑战性的生物系统中固态 NMR 光谱中 H-1 检测的 HSQC
DOI：
10.1002/chem.201805327
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发表时间：
2019
期刊：
影响因子：
--
通讯作者：
Wang Shenlin
中科院分区：
文献类型：
--
作者：
Han Rong;Yang Yufei;Wang Shenlin
固态（SS）NMR光谱是研究具有挑战性的生物系统的强大技术，但它通常具有低灵敏度。报道了一种提高固体核磁共振HSQC实验信号灵敏度的纵向弛豫优化方案。在该方案下，选择1H-X（15 N或13 C）的1H自旋进行信号采集，而将其他较大的1H自旋翻转回静磁场的轴，以加速被翻转的1H自旋的自旋恢复，从而提高灵敏度。使用三种生物系统来评估这种策略，包括七跨膜蛋白、RNA和全细胞样品。对于所有三种样品，所提出的方案大大缩短了有效的1H纵向弛豫时间，并导致灵敏度提高1.3-2.5倍。所选系统是具有挑战性的生物系统，通过SSNMR光谱观察的代表，从而表明这种方法的普遍适用性，这是特别重要的生物样品的寿命短或有限的样品量。
Solid‐state (SS) NMR spectroscopy is a powerful technique for studying challenging biological systems, but it often suffers from low sensitivity. A longitudinal relaxation optimization scheme to enhance the signal sensitivity of HSQC experiments in SSNMR spectroscopy is reported. Under the proposed scheme, the1H spins of1H–X (15N or13C) are selected for signal acquisition, whereas other vast1H spins are flipped back to the axis of the static magnetic field to accelerate the spin recovery of the observed1H spins, resulting in enhanced sensitivity. Three biological systems are used to evaluate this strategy, including a seven‐transmembrane protein, an RNA, and a whole‐cell sample. For all three samples, the proposed scheme largely shortens the effective1H longitudinal relaxation time and results in a 1.3–2.5‐fold gain in sensitivity. The selected systems are representative of challenging biological systems for observation by means of SSNMR spectroscopy; thus indicating the general applicability of this method, which is particularly important for biological samples with a short lifetime or with limited sample quantities.