Francis Bitter Magnet Laboratory and Department of Chemistry, Cambridge, MA 02139, USA.
Phys Chem Chem Phys. 2010 Jun 14;12(22):5872-8. doi: 10.1039/c003705b. Epub 2010 May 11.
Perdeuteration of biological macromolecules for magic angle spinning solid-state NMR spectroscopy can yield high-resolution (2)H-(13)C 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 (2)H-(13)C correlation spectra with a signal enhancement of epsilon > or = 700 compared to a spectrum recorded with microwaves off and otherwise identical conditions. To our knowledge, this is the first time that (2)H-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 (2)H-(13)C correlation spectra of U-[(2)H, (13)C] proline.
对生物大分子进行去氘化处理，可用于魔角旋转固态 NMR 光谱学，从而得到高分辨率的 (2)H-(13)C 相关谱，因此该方法受到结构生物学界的广泛关注。在这里，我们证明了样品去氘化和动态核极化的结合，可以得到分辨的 (2)H-(13)C 相关谱，与在微波关闭且其他条件相同的情况下记录的谱相比，信号增强了 epsilon >或= 700。据我们所知，这是首次将 (2)H-DNP 用于增强与生物学相关系统的 MAS-NMR 谱。该 DNP 过程使用几种极化剂进行研究，并将该技术应用于获得 U-[(2)H, (13)C]脯氨酸的 (2)H-(13)C 相关谱。
