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
相关论文
共 55 条
[31]   High-resolution 1H NMR in the solid state using symmetry-based pulse sequences [J].
Madhu, PK ;
Zhao, X ;
Levitt, MH .
CHEMICAL PHYSICS LETTERS, 2001, 346 (1-2) :142-148
[32]  
MCDERMOTT A, 1997, ENCY NMR, P3820
[33]   1H-1H MAS correlation spectroscopy and distance measurements in a deuterated peptide [J].
Reif, B ;
Jaroniec, CP ;
Rienstra, CM ;
Hohwy, M ;
Griffin, RG .
JOURNAL OF MAGNETIC RESONANCE, 2001, 151 (02) :320-327
[34]   ANALYSIS OF MULTIPLE PULSE NMR IN SOLIDS [J].
RHIM, WK ;
ELLEMAN, DD ;
VAUGHAN, RW .
JOURNAL OF CHEMICAL PHYSICS, 1973, 59 (07) :3740-3749
[35]   Recoupled polarization transfer heteronuclear 1H-13C multiple-quantum correlation in solids under ultra-fast MAS [J].
Saalwächter, K ;
Graf, R ;
Spiess, HW .
JOURNAL OF MAGNETIC RESONANCE, 1999, 140 (02) :471-476
[36]   Recoupled polarization-transfer methods for solid-state 1H-13C heteronuclear correlation in the limit of fast MAS [J].
Saalwächter, K ;
Graf, R ;
Spiess, HW .
JOURNAL OF MAGNETIC RESONANCE, 2001, 148 (02) :398-418
[37]   Heteronuclear 1H-13C multiple-spin correlation in solid-state nuclear magnetic resonance:: Combining rotational-echo double-resonance recoupling and multiple-quantum spectroscopy [J].
Saalwächter, K ;
Spiess, HW .
JOURNAL OF CHEMICAL PHYSICS, 2001, 114 (13) :5707-5728
[38]   The effect of spin decoupling on line shapes in solid-state nuclear magnetic resonance [J].
Sachleben, JR ;
Caldarelli, S ;
Emsley, L .
JOURNAL OF CHEMICAL PHYSICS, 1996, 104 (07) :2518-2528
[39]   Homonuclear dipolar decoupling in solid-state NMR using continuous phase modulation [J].
Sakellariou, D ;
Lesage, A ;
Hodgkinson, P ;
Emsley, L .
CHEMICAL PHYSICS LETTERS, 2000, 319 (3-4) :253-260
[40]   Proton-proton constraints in powdered solids from 1H-1H-1H and 1H-1H-13C three-dimensional NMR chemical shift correlation spectroscopy [J].
Sakellariou, D ;
Lesage, A ;
Emsley, L .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2001, 123 (23) :5604-5605