High-resolution 1H homonuclear dipolar recoupling NMR spectra of biological solids at MAS rates up to 67 kHz

被引：59

作者：

Mafra, Luis ^{[1
]}

Siegel, Renee ^{[1
]}

Fernandez, Christian ^{[2
]}

Schneider, Denis ^{[3
]}

Aussenac, Fabien ^{[4
]}

Rocha, Joao ^{[1
]}

机构：

[1] Univ Aveiro, Dept Chem, CICECO, P-3810193 Aveiro, Portugal

[2] Univ Caen, ENSICAEN, Lab Catalyse & Spectrochim, CNRS, F-14050 Caen, France

[3] Bruker Biospin GMBH, D-76287 Rheinstetten, Germany

[4] Bruker Biospin SA, F-67166 Wissembourg, France

来源：

JOURNAL OF MAGNETIC RESONANCE | 2009年 / 199卷 / 01期

关键词：

High-resolution solid-state H-1 NMR; Ultra-fast MAS; H-1-H-1; decoupling; CRAMPS; 2D H-1-H-1 single-quantum-double-quantum spectra; wDUMBO; Double-quantum recoupling; Homonuclear correlation; Rotor-synchronised symmetry sequences; NUCLEAR-MAGNETIC-RESONANCE; PULSE SEQUENCES; MULTIPLE-PULSE; STATE; ANGLE; SPECTROSCOPY; EXCITATION; RECOVERY; FIELD;

D O I：

10.1016/j.jmr.2009.04.004

中图分类号：

Q5 [生物化学];

学科分类号：

071010 ; 081704 ;

摘要：

Two-dimensional H-1 homonuclear correlation NMR spectra of solids of biological interest have been recorded at high magnetic fields (14.1 and 18.8 T) and MAS rates up to 67 kHz, using RNnv symmetry-based homonuclear recoupling and CRAMPS decoupling; this method affords exceptional spectral resolution and is well suited to probe H-1-H-1 proximities in powdered solids. (C) 2009 Elsevier Inc. All rights reserved.

引用

页码：111 / 114

页数：4

共 24 条

[1] High-order multiple quantum excitation in 13C nuclear magnetic resonance spectroscopy of organic solids [J].

Antzutkin, ON ;

Tycko, R .

JOURNAL OF CHEMICAL PHYSICS, 1999, 110 (06) :2749-2752

[2]

BEEK JD, 2000, NATURE, V405, P1077

[3] FREQUENCY-SWITCHED PULSE SEQUENCES - HOMONUCLEAR DECOUPLING AND DILUTE SPIN NMR IN SOLIDS [J].

BIELECKI, A ;

KOLBERT, AC ;

LEVITT, MH .

CHEMICAL PHYSICS LETTERS, 1989, 155 (4-5) :341-346

[4] Probing proton-proton proximities in the solid state:: High-resolution two-dimensional 1H-1H double-quantum CRAMPS NMR spectroscopy [J].

Brown, SP ;

Lesage, A ;

Elena, B ;

Emsley, L .

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2004, 126 (41) :13230-13231

[5] LOW-POWER MULTIPULSE LINE NARROWING IN SOLID-STATE NMR [J].

BURUM, DP ;

LINDER, M ;

ERNST, RR .

JOURNAL OF MAGNETIC RESONANCE, 1981, 44 (01) :173-188

[6] Symmetry principles for the design of radiofrequency pulse sequences in the nuclear magnetic resonance of rotating solids [J].

Carravetta, M ;

Edén, M ;

Zhao, X ;

Brinkmann, A ;

Levitt, MH .

CHEMICAL PHYSICS LETTERS, 2000, 321 (3-4) :205-215

[7] Excitation of carbon-13 triple quantum coherence in magic-angle-spinning NMR [J].

Eden, M ;

Levitt, MH .

CHEMICAL PHYSICS LETTERS, 1998, 293 (3-4) :173-179

[8] Direct determination of a molecular torsional angle in the membrane protein rhodopsin by solid-state NMR [J].

Feng, X ;

Verdegem, PJE ;

Lee, YK ;

Sandstrom, D ;

Eden, M ;

BoveeGeurts, P ;

deGrip, WJ ;

Lugtenburg, J ;

deGroot, HJM ;

Levitt, MH .

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1997, 119 (29) :6853-6857

[9] Site-resolved determination of peptide torsion angle phi from the relative orientations of backbone N-H and C-H bonds by solid-state NMR [J].

Hong, M ;

Gross, JD ;

Griffin, RG .

JOURNAL OF PHYSICAL CHEMISTRY B, 1997, 101 (30) :5869-5874

[10] Double-quantum dipolar recoupling at high magic-angle spinning rates [J].

Kristiansen, PE ;

Mitchell, DJ ;

Evans, JNS .

JOURNAL OF MAGNETIC RESONANCE, 2002, 157 (02) :253-266

← 1 2 3 →