1H detection in MAS solid-state NMR Spectroscopy of biomacromolecules employing pulsed field gradients for residual solvent suppression
1H detection in MAS solid-state NMR Spectroscopy of biomacromolecules employing pulsed field gradients for residual solvent suppression
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DOI：
10.1021/ja029354b
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发表时间：
2003-07-02
影响因子：
15
通讯作者：
Reif, B
中科院分区：
文献类型：
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作者：
Chevelkov, V;van Rossum, BJ;Reif, B
在这篇文章中，我们证明了利用脉冲场梯度抑制水磁化，在MAS固态核磁共振中对鸡α-谱蛋白SH3结构域的微晶、均匀2h、15n标记样品进行1h检测的可行性。今天，在溶液态核磁共振中，通常使用b梯度进行相干顺序选择和溶剂抑制。我们建议使用梯度来清除水磁化，而传统的水抑制方案无法抑制水磁化。与实验的15n检测版本（MAS旋转频率为13.5 kHz）相比，1h检测可实现的灵敏度增益约为5。我们期望这种由于1H检测而达到高灵敏度的标记概念，结合我们之前所展示的测量长距离1H - 1H距离的可能性，成为测定固态蛋白质结构的有用工具。
In this communication, we demonstrate the feasibility of1H detection in MAS solid-state NMR for a microcrystalline, uniformly2H,15N-labeled sample of a SH3 domain of chicken α-spectrin, using pulsed field gradients for suppression of water magnetization. Today,B0gradients are employed routinely in solution-state NMR for coherence order selection and solvent suppression. We suggest to use gradients to purge water magnetization which cannot be suppressed using conventional water suppression schemes. The achievable gain in sensitivity for1H detection is in the order of 5 compared to the15N detected version of the experiment (at a MAS rotation frequency of 13.5 kHz). We expect that this labeling concept which achieves high sensitivity due to1H detection, in combination with the possibility to measure long range1H−1H distances as we have shown previously, to be a useful tool for the determination of protein structures in the solid state.