DNP 增强的细菌视紫红质中频率选择 TEDOR 实验。
DNP enhanced frequency-selective TEDOR experiments in bacteriorhodopsin.
机构信息
Department of Chemistry, Massachusetts Institute of Technology, Cambridge, MA 02139, USA.
出版信息
J Magn Reson. 2010 Jan;202(1):9-13. doi: 10.1016/j.jmr.2009.09.005. Epub 2009 Sep 9.
Abstract
We describe a new approach to multiple (13)C-(15)N distance measurements in uniformly labeled solids, frequency-selective (FS) TEDOR. The method shares features with FS-REDOR and ZF- and BASE-TEDOR, which also provide quantitative (15)N-(13)C spectral assignments and distance measurements in U-[(13)C,(15)N] samples. To demonstrate the validity of the FS-TEDOR sequence, we measured distances in [U-(13)C,(15)N]-asparagine which are in good agreement with other methods. In addition, we integrate high frequency dynamic nuclear polarization (DNP) into the experimental protocol and use FS-TEDOR to record a resolved correlation spectrum of the Arg-(13)C(gamma)-(15)N(epsilon) region in [U-(13)C,(15)N]-bacteriorhodopsin. We resolve six of the seven cross-peaks expected based on the primary sequence of this membrane protein.
摘要
我们描述了一种在均标记固体中进行多个（13）C-（15）N 距离测量的新方法，即频率选择（FS）TEDOR。该方法与 FS-REDOR 和 ZF- 和 BASE-TEDOR 具有共同的特点，这两种方法也可在 U-[(13)C,（15）N]样品中提供定量（15）N-（13）C 光谱分配和距离测量。为了证明 FS-TEDOR 序列的有效性，我们测量了 [U-（13）C，（15）N]-天冬酰胺中的距离，这些距离与其他方法非常吻合。此外，我们将高频动态核极化（DNP）集成到实验方案中，并使用 FS-TEDOR 记录 [U-（13）C，（15）N]-细菌视紫红质中 Arg-（13）C（γ）-（15）N（ε）区域的分辨相关谱。我们根据该膜蛋白的一级序列解析了七个预期的交叉峰中的六个。
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