Perras, F.A., T. Kobayashi, and M. Pruski, Natural Abundance (17)O DNP Two-Dimensional and Surface-Enhanced NMR Spectroscopy. J Am Chem Soc, 2015. 137(26): p. 8336-9.
Due to its extremely low natural abundance and quadrupolar nature, the (17)O nuclide is very rarely used for spectroscopic investigation of solids by NMR without isotope enrichment. Additionally, the applicability of dynamic nuclear polarization (DNP), which leads to sensitivity enhancements of 2 orders of magnitude, to (17)O is wrought with challenges due to the lack of spin diffusion and low polarization transfer efficiency from (1)H. Here, we demonstrate new DNP-based measurements that extend (17)O solid-state NMR beyond its current capabilities. The use of the PRESTO technique instead of conventional (1)H-(17)O cross-polarization greatly improves the sensitivity and enables the facile measurement of undistorted line shapes and two-dimensional (1)H-(17)O HETCOR NMR spectra as well as accurate internuclear distance measurements at natural abundance. This was applied for distinguishing hydrogen-bonded and lone (17)O sites on the surface of silica gel; the one-dimensional spectrum of which could not be used to extract such detail. Lastly, this greatly enhanced sensitivity has enabled, for the first time, the detection of surface hydroxyl sites on mesoporous silica at natural abundance, thereby extending the concept of DNP surface-enhanced NMR spectroscopy to the (17)O nuclide.
Natural Abundance 17O DNP Two-Dimensional and Surface-Enhanced NMR Spectroscopy
Natural Abundance 17O DNP Two-Dimensional and Surface-Enhanced NMR Spectroscopy
Fre?de?ric A. Perras, Takeshi Kobayashi and Marek Pruski
http://pubs.acs.org/appl/literatum/publisher/achs/journals/content/jacsat/0/jacsat.ahead-of-print/jacs.5b03905/20150629/images/medium/ja-2015-03905b_0003.gif
Journal of the American Chemical Society
DOI: 10.1021/jacs.5b03905
http://feeds.feedburner.com/~ff/acs/jacsat?d=yIl2AUoC8zA
http://feeds.feedburner.com/~r/acs/jacsat/~4/2XY9E0YdGEg
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06-29-2015 07:21 PM
Matrix-free dynamic nuclear polarization enables solid-state NMR (13)C-(13)C correlation spectroscopy of proteins at natural isotopic abundance
From The DNP-NMR Blog:
Matrix-free dynamic nuclear polarization enables solid-state NMR (13)C-(13)C correlation spectroscopy of proteins at natural isotopic abundance
Takahashi, H., S. Hediger, and G. De Paepe, Matrix-free dynamic nuclear polarization enables solid-state NMR (13)C-(13)C correlation spectroscopy of proteins at natural isotopic abundance. Chem Commun (Camb), 2013. 49(82): p. 9479-81.
http://www.ncbi.nlm.nih.gov/pubmed/24013616
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11-21-2013 01:14 AM
[NMR paper] Matrix-free dynamic nuclear polarization enables solid-state NMR (13)C-(13)C correlation spectroscopy of proteins at natural isotopic abundance.
Matrix-free dynamic nuclear polarization enables solid-state NMR (13)C-(13)C correlation spectroscopy of proteins at natural isotopic abundance.
Matrix-free dynamic nuclear polarization enables solid-state NMR (13)C-(13)C correlation spectroscopy of proteins at natural isotopic abundance.
Chem Commun (Camb). 2013 Sep 6;
Authors: Takahashi H, Hediger S, De Paëpe G
Abstract
We introduce a general approach for dynamic nuclear polarization (DNP) enhanced solid-state NMR that overcomes the current problems in DNP experiments caused by the use...
Dynamic Nuclear Polarization Enhanced Natural Abundance 17O Spectroscopy
From the The DNP-NMR Blog:
Dynamic Nuclear Polarization Enhanced Natural Abundance 17O Spectroscopy
Blanc, F., et al., Dynamic Nuclear Polarization Enhanced Natural Abundance 17O Spectroscopy. J. Am. Chem. Soc., 2013. 135(8): p. 2975-2978.
http://dx.doi.org/10.1021/ja4004377
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04-15-2013 08:52 AM
Identifying Guanosine Self Assembly at Natural Isotopic Abundance by High-Resolution 1H and 13C Solid-State NMR Spectroscopy
Identifying Guanosine Self Assembly at Natural Isotopic Abundance by High-Resolution 1H and 13C Solid-State NMR Spectroscopy
Amy L. Webber, Stefano Masiero, Silvia Pieraccini, Jonathan C. Burley, Andrew S. Tatton, Dinu Iuga, Tran N. Pham, Gian Piero Spada and Steven P. Brown
http://pubs.acs.org/appl/literatum/publisher/achs/journals/content/jacsat/0/jacsat.ahead-of-print/ja206516u/aop/images/medium/ja-2011-06516u_0007.gif
Journal of the American Chemical Society
DOI: 10.1021/ja206516u
http://feeds.feedburner.com/~ff/acs/jacsat?d=yIl2AUoC8zA...
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11-18-2011 04:35 AM
Surface Enhanced NMR Spectroscopy by Dynamic Nuclear Polarization
Surface Enhanced NMR Spectroscopy by Dynamic Nuclear Polarization
Anne Lesage, Moreno Lelli, David Gajan, Marc A. Caporini, Veronika Vitzthum, Pascal Mie?ville, Johan Alauzun, Arthur Roussey, Chloe? Thieuleux, Ahmad Medhi, Geoffrey Bodenhausen, Christophe Cope?ret and Lyndon Emsley
http://pubs.acs.org/appl/literatum/publisher/achs/journals/content/jacsat/0/jacsat.ahead-of-print/ja104771z/aop/images/medium/ja-2010-04771z_0004.gif
Journal of the American Chemical Society
DOI: 10.1021/ja104771z
http://feeds.feedburner.com/~ff/acs/jacsat?d=yIl2AUoC8zA...