A magic angle spinning (MAS) NMR technique to transfer polarization from protons to a specific set of the C-13 spins is introduced for the study of biomolecular samples in the solid-state. Ultrafast (>60 kHz) MAS and low irradiation rf fields are used to achieve band-selective Hartmann-Hahn cross-polarization (CP) between the whole proton bath and carbons whose resonances are close to the C-13-transmitter offset. When compared to conventional, broadband H-1-C-13 CP, the band-selective experiment can be established without any loss of sensitivity when polarizing the aliphatic signals of a protein sample, and with a significant gain when polarizing carbonyls, This scheme can be used as a building block in 2D C-13-C-13 homonuclear correlation experiments to obtain a faster and more sensitive characterization of biological solids.

Band-selective 1H-13C cross-polarization in fast magic angle spinning solid-state NMR spectroscopy / S. Laage; A. Marchetti; J. Sein; R. Pierattelli; H.J. Sass; S. Grzesiek; A. Lesage; G. Pintacuda; L. Emsley. - In: JOURNAL OF THE AMERICAN CHEMICAL SOCIETY. - ISSN 0002-7863. - STAMPA. - 130:(2008), pp. 17216-17217. [10.1021/ja805926d]

Band-selective 1H-13C cross-polarization in fast magic angle spinning solid-state NMR spectroscopy

PIERATTELLI, ROBERTA;
2008

Abstract

A magic angle spinning (MAS) NMR technique to transfer polarization from protons to a specific set of the C-13 spins is introduced for the study of biomolecular samples in the solid-state. Ultrafast (>60 kHz) MAS and low irradiation rf fields are used to achieve band-selective Hartmann-Hahn cross-polarization (CP) between the whole proton bath and carbons whose resonances are close to the C-13-transmitter offset. When compared to conventional, broadband H-1-C-13 CP, the band-selective experiment can be established without any loss of sensitivity when polarizing the aliphatic signals of a protein sample, and with a significant gain when polarizing carbonyls, This scheme can be used as a building block in 2D C-13-C-13 homonuclear correlation experiments to obtain a faster and more sensitive characterization of biological solids.
2008
130
17216
17217
S. Laage; A. Marchetti; J. Sein; R. Pierattelli; H.J. Sass; S. Grzesiek; A. Lesage; G. Pintacuda; L. Emsley
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Utilizza questo identificatore per citare o creare un link a questa risorsa: https://hdl.handle.net/2158/345103
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