Hyperpolarization of NMR-active nuclei is key to gather high quality spectra of rare species and insensitive isotopes. We have recently established that silica-based materials containing regularly distributed nitroxyl radicals connected to the silica matrix by flexible linkers can serve as promising polarization matrices in DNP. Here we investigate the influence of the linker on the efficiency of the polarization. The materials were fully characterized and exhibit high surface areas and narrow pore size distributions with a tunable amount of phenyl azide groups over a broad range of concentrations. The phenyl azide groups can be easily functionalized via a two-step procedure into 4-carboxy-2,2,6,6-tetramethyl-1-oxyl-piperidine (TEMPO) to give polarizing matrices with controllable radical content. The DNP efficiency was found to be similar as in materials with flexible linkers, both for MAS at 105 K and dissolution DNP at 4 K. This article is protected by copyright. All rights reserved.
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Essentials of Dynamic Nuclear Polarization #DNPNMR
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Essentials of Dynamic Nuclear Polarization #DNPNMR
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Reverse micelles as a platform for dynamic nuclear polarization in solution NMR of proteins
From The DNP-NMR Blog:
Reverse micelles as a platform for dynamic nuclear polarization in solution NMR of proteins
Valentine, K.G., et al., Reverse micelles as a platform for dynamic nuclear polarization in solution NMR of proteins. J Am Chem Soc, 2014. 136(7): p. 2800-7.
http://pubs.acs.org/doi/abs/10.1021/ja4107176
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03-27-2014 03:46 AM
[NMR paper] Reverse micelles as a platform for dynamic nuclear polarization in solution NMR of proteins.
Reverse micelles as a platform for dynamic nuclear polarization in solution NMR of proteins.
Related Articles Reverse micelles as a platform for dynamic nuclear polarization in solution NMR of proteins.
J Am Chem Soc. 2014 Jan 24;
Authors: Valentine KG, Mathies G, Bédard S, Nucci NV, Dodevski I, Stetz MA, Can TV, Griffin RG, Wand AJ
Abstract
Despite tremendous advances in recent years, solution NMR remains fundamentally restricted due to its inherent insensitivity. Dynamic nuclear polarization (DNP) potentially offers significant...