2H-DNP-enhanced 2H-13C solid-state NMR correlation spectroscopy.

2H-DNP-enhanced 2H-13C solid-state NMR correlation spectroscopy.
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2H-DNP 增强 2H-13C 固态 NMR 相关光谱。

DOI:
10.1039/c003705b
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发表时间:
2010
期刊:
Physical chemistry chemical physics : PCCP
影响因子:
--
通讯作者:
Griffin,RobertG
Griffin,RobertG
中科院分区:
--
文献类型:
--
作者:
Maly,Thorsten;Andreas,LorenB;Smith,AlbertA;Griffin,RobertG

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魔角旋转固体核磁共振法用于生物大分子的全氚化能获得高分辨率的2H-13C相关谱,因此引起了结构生物界的极大兴趣。在这里,我们证明了样品氚和动态核极化产额的结合,分辨了2H-13C相关谱,与用微波关闭和其他相同条件下记录的谱相比,信号增强了ε≥700。据我们所知,这是首次使用2H-DNP来增强生物相关体系的MAS-核磁共振谱。用几种偏振剂研究了DNP过程,并应用该技术获得了U-[2H,13C]Pro的2H-13C相关谱。
Perdeuteration of biological macromolecules for magic angle spinning solid-state NMR spectroscopy can yield high-resolution 2H–13C correlation spectra and the method is therefore of great interest for the structural biology community. Here we demonstrate that the combination of sample deuteration and dynamic nuclear polarization yields resolved 2H–13C correlation spectra with a signal enhancement of ε ≥ 700 compared to a spectrum recorded with microwaves off and otherwise identical conditions. To our knowledge, this is the first time that 2H-DNP has been employed to enhance MAS-NMR spectra of a biologically relevant system. The DNP process is studied using several polarizing agents and the technique is applied to obtain 2H–13C correlation spectra of U-[2H, 13C] proline.
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