利用固态核磁共振波谱法从生物固体中的距离和取向约束确定全局结构

Determination of global structure from distance and orientation constraints in biological solids using solid-state NMR spectroscopy.

作者信息

Andreas Loren B, Mehta Anil K, Mehta Manish A

机构信息

Department of Chemistry and Biochemistry, Oberlin College, Oberlin, Ohio 44074, USA.

出版信息

J Am Chem Soc. 2007 Dec 12;129(49):15233-9. doi: 10.1021/ja074789q. Epub 2007 Nov 9.

DOI:10.1021/ja074789q

PMID:17990880

Abstract

We report the results from a new solid-state NMR experiment, DANTE-REDOR, which can determine global secondary structure in uniformly (13C,15N)-enriched systems by simultaneously measuring distance and orientation constraints. Following a heteronuclear spin-pair selection using a DANTE pulse train, the magnitude and orientation of the internuclear dipole vector, within the chemical shift anisotropy (CSA) frame of the observed nucleus, are determined by tracking the dephasing of individual spinning sidebands under magic angle spinning. The efficacy of the experiment is demonstrated by measuring the imidazole side-chain orientation in U-[13C6,15N3]-L-histidine x HCl x H2O.

摘要

我们报告了一种新的固态核磁共振实验——DANTE-REDOR的结果，该实验可通过同时测量距离和取向约束来确定均匀（13C，15N）富集体系中的整体二级结构。在使用DANTE脉冲序列进行异核自旋对选择之后，通过跟踪魔角旋转下各个旋转边带的去相位，在观测核的化学位移各向异性（CSA）框架内确定核间偶极矢量的大小和取向。通过测量U-[13C6,15N3]-L-组氨酸x HCl x H2O中咪唑侧链的取向，证明了该实验的有效性。