Rapid Natural-Abundance 2D 13C-13C Correlation Spectroscopy Using Dynamic Nuclear Polarization Enhanced Solid-State NMR and Matrix-Free Sample Preparation

被引：153

作者：

Takahashi, Hiroki ^{[1
,2
]}

Lee, Daniel ^{[1
,2
]}

Dubois, Lionel ^{[1
,2
]}

Bardet, Michel ^{[1
,2
]}

Hediger, Sabine ^{[1
,2
]}

De Paepe, Gael ^{[1
,2
]}

机构：

[1] UMR E3 CEA UJF, Lab Chim Inorgan & Biol, F-38054 Grenoble, France

[2] Inst Nanosci & Cryogenie CEA DSM, CNRS, F-38054 Grenoble, France

来源：

ANGEWANDTE CHEMIE-INTERNATIONAL EDITION | 2012年 / 51卷 / 47期

关键词：

2D correlation; analytical methods; dynamic nuclear polarization; natural abundance; NMR spectroscopy; RESONANCE; MEMBRANES; PROTEINS;

D O I：

10.1002/anie.201206102

中图分类号：

O6 [化学];

学科分类号：

0703 ;

摘要：

Ultra-fast: Substantial solid-state NMR sensitivity can be achieved using dynamic nuclear polarization and matrix-free sample preparation (that is, absence of solvent and cryoprotectant). This method avoids line-broadening, maximizes sample filling factor, and allows natural-abundance 2D 13C-13C dipolar correlation experiments to be carried out in tens of minutes. MW=microwaves. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

引用

页码：11766 / 11769

页数：4

共 30 条

[1]

Akbey U., 2010, ANGEW CHEM, V122, P7971

[2] Dynamic Nuclear Polarization of Deuterated Proteins [J].

Akbey, Uemit ;

Franks, W. Trent ;

Linden, Arne ;

Lange, Sascha ;

Griffin, Robert G. ;

van Rossum, Barth-Jan ;

Oschkinat, Hartmut .

ANGEWANDTE CHEMIE-INTERNATIONAL EDITION, 2010, 49 (42) :7803-7806

[3] Functional and shunt states of bacteriorhodopsin resolved by 250 GHz dynamic nuclear polarization-enhanced solid-state NMR [J].

Bajaj, Vikram S. ;

Mak-Jurkauskas, Melody L. ;

Belenky, Marina ;

Herzfeld, Judith ;

Griffin, Robert G. .

PROCEEDINGS OF THE NATIONAL ACADEMY OF SCIENCES OF THE UNITED STATES OF AMERICA, 2009, 106 (23) :9244-9249

[4] Dynamic nuclear polarization at 9T using a novel 250 GHz gyrotron microwave source [J].

Bajaj, VS ;

Farrar, CT ;

Hornstein, MK ;

Mastovsky, I ;

Vieregg, J ;

Bryant, J ;

Eléna, B ;

Kreischer, KE ;

Temkin, RJ ;

Griffin, RG .

JOURNAL OF MAGNETIC RESONANCE, 2003, 160 (02) :85-90

[5] Transverse dephasing optimised NMR spectroscopy in solids:: Natural-abundance 13C correlation spectra [J].

De Paëpe, G ;

Lesage, A ;

Steuernagel, S ;

Emsley, L .

CHEMPHYSCHEM, 2004, 5 (06) :869-875

[6] Polarization-enhanced NMR spectroscopy of biomolecules in frozen solution [J].

Hall, DA ;

Maus, DC ;

Gerfen, GJ ;

Inati, SJ ;

Becerra, LR ;

Dahlquist, FW ;

Griffin, RG .

SCIENCE, 1997, 276 (5314) :930-932

[7] Broadband dipolar recoupling in the nuclear magnetic resonance of rotating solids:: A compensated C7 pulse sequence [J].

Hohwy, M ;

Jakobsen, HJ ;

Edén, M ;

Levitt, MH ;

Nielsen, NC .

JOURNAL OF CHEMICAL PHYSICS, 1998, 108 (07) :2686-2694

[8] Characterization of Membrane Proteins in Isolated Native Cellular Membranes by Dynamic Nuclear Polarization Solid-State NMR Spectroscopy without Purification and Reconstitution [J].

Jacso, Tomas ;

Franks, W. Trent ;

Rose, Honor ;

Fink, Uwe ;

Broecker, Jana ;

Keller, Sandro ;

Oschkinat, Hartmut ;

Reif, Bernd .

ANGEWANDTE CHEMIE-INTERNATIONAL EDITION, 2012, 51 (02) :432-435

[9]

Jacso Tomas., 2012, Angewandte Chemie International Edition, V124, P447, DOI [DOI 10.1002/ANGE.201104987, 10.1002/ange.201104987]

[10] Determination of the through-bond carbon-carbon and carbon-proton connectivities of the native celluloses in the solid state [J].

Kono, H ;

Erata, T ;

Takai, M .

MACROMOLECULES, 2003, 36 (14) :5131-5138

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