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

被引:155
作者
Lesage, A
Sakellariou, D
Hediger, S
Eléna, B
Charmont, P
Steuernagel, S
Emsley, L [1 ]
机构
[1] Ecole Normale Super Lyon, CEA, Lab Rech Conventionne 23V, CNRS,ENS,Lab Chim, F-69364 Lyon, France
[2] Univ Calif Berkeley, Dept Chem, Berkeley, CA 94720 USA
[3] Bruker BioSpin GmbH, D-76287 Rheinstetten, Germany
关键词
solid-state proton spectroscopy; high-field NMR; homonuclear decoupling; fast MAS; heteronuclear spectroscopy;
D O I
10.1016/S1090-7807(03)00104-6
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
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 H-1 dimension. An example is provided with the C-13-H-1 MAS-J-HMQC experiment. (C) 2003 Elsevier Science (USA). All rights reserved.
引用
收藏
页码:105 / 113
页数:9
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