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使用相位调制同核偶极去耦的固体质子核磁共振光谱的实验方面。

Experimental aspects of proton NMR spectroscopy in solids using phase-modulated homonuclear dipolar decoupling.

作者信息

Lesage Anne, Sakellariou Dimitris, Hediger Sabine, Eléna Bénédicte, Charmont Patrick, Steuernagel Stefan, Emsley Lyndon

机构信息

UMR-5532 CNRS/ENS, Laboratoire de Recherche Conventionné du CEA (23V), Ecole Normale Supérieure de Lyon, 69364 Lyon, France.

出版信息

J Magn Reson. 2003 Jul;163(1):105-13. doi: 10.1016/s1090-7807(03)00104-6.

Abstract

In this paper we demonstrate experimentally that the continuously phase-modulated homonuclear decoupling sequence DUMBO-1 is suitable for high-resolution proton NMR spectroscopy of rigid solids. Over a wide range of experimental conditions, we show on the model sample L-alanine as well as on small peptides that proton linewidths of less than 0.5 ppm can be obtained under DUMBO-1 decoupling. In particular the DUMBO-1 sequence yields well resolved proton spectra both at slow and fast MAS. The DUMBO-1 decoupling scheme can in principle be inserted in any multi-nuclear or multi-dimensional solid-state NMR experiment which requires a high-resolution 1H dimension. An example is provided with the 13C-1H MAS-J-HMQC experiment.

摘要

在本文中,我们通过实验证明,连续相位调制的同核去耦序列DUMBO-1适用于刚性固体的高分辨率质子核磁共振光谱分析。在广泛的实验条件下,我们在模型样品L-丙氨酸以及小肽上表明,在DUMBO-1去耦条件下可以获得小于0.5 ppm的质子线宽。特别是,DUMBO-1序列在慢速和快速MAS条件下都能产生分辨率良好的质子光谱。DUMBO-1去耦方案原则上可以插入任何需要高分辨率1H维度的多核或多维固态核磁共振实验中。以13C-1H MAS-J-HMQC实验为例进行了说明。

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