A recent study explored the use of hyperpolarized water, to enhance the sensitivity of nuclei in biomolecules thanks to rapid proton exchanges with labile amide backbone and sidechain groups. Further optimizations of this approach have now allowed us to achieve proton polarizations approaching 25% in the water transferred into the NMR spectrometer, effective water T1 times approaching 40s, and a reduction in the dilution demanded for the cryogenic dissolution process. Further hardware developments have allowed us to perform these experiments, repeatedly and reliably, in 5mm NMR tubes. All these ingredients - particularly the 3000x (1)H polarization enhancements over 11.7T thermal counterparts, long T1 times and a compatibility with high-resolution biomolecular NMR setups - augur well for hyperpolarized 2D NMR studies of peptides, unfolded proteins and intrinsically disordered systems undergoing fast exchanges of their protons with the solvent. This hypothesis is here explored by detailing the provisions that lead to these significant improvements over previous reports, and demonstrating 1D coherence transfer experiments and 2D biomolecular HMQC acquisitions delivering NMR spectral enhancements of 100-500x over their optimized, thermally-polarized, counterparts.
Optimizing dissolution dynamic nuclear polarization
From The DNP-NMR Blog:
Optimizing dissolution dynamic nuclear polarization
Bornet, A. and S. Jannin, Optimizing dissolution dynamic nuclear polarization. J Magn Reson, 2016. 264: p. 13-21.
http://www.ncbi.nlm.nih.gov/pubmed/26920826
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04-26-2016 12:03 AM
[NMR paper] Optimizing water hyperpolarization and dissolution for sensitivity-enhanced 2D biomolecular NMR.
Optimizing water hyperpolarization and dissolution for sensitivity-enhanced 2D biomolecular NMR.
Optimizing water hyperpolarization and dissolution for sensitivity-enhanced 2D biomolecular NMR.
J Magn Reson. 2016 Mar;264:49-58
Authors: Olsen G, Markhasin E, Szekely O, Bretschneider C, Frydman L
Abstract
A recent study explored the use of hyperpolarized water, to enhance the sensitivity of nuclei in biomolecules thanks to rapid proton exchanges with labile amide backbone and sidechain groups. Further optimizations of this...
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02-28-2016 03:10 PM
[NMR paper] Optimizing water hyperpolarization and dissolution for sensitivity-enhanced 2D biomolecular NMR
Optimizing water hyperpolarization and dissolution for sensitivity-enhanced 2D biomolecular NMR
Publication date: March 2016
Source:Journal of Magnetic Resonance, Volume 264</br>
Author(s): Greg Olsen, Evgeny Markhasin, Or Szekely, Christian Bretschneider, Lucio Frydman</br>
A recent study explored the use of hyperpolarized water, to enhance the sensitivity of nuclei in biomolecules thanks to rapid proton exchanges with labile amide backbone and sidechain groups. Further optimizations of this approach have now allowed us to achieve proton polarizations...
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02-24-2016 01:30 AM
Into the fold: Sensitivity-enhanced NMR
Into the fold: Sensitivity-enhanced NMR
http://www.spectroscopynow.com/common/images/thumbnails/15061c31a88.jpgResearchers at Massachusetts Institute of Technology have used sensitivity-enhanced nuclear magnetic resonance (NMR) spectroscopy to analyse the structure that a yeast protein forms as it interacts with other proteins in a cell opening up new insights into protein folding and misfolding.
Read the rest at Spectroscopynow.com
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10-15-2015 12:19 PM
[NMR paper] A comparison of chemical shift sensitivity of trifluoromethyl tags: optimizing resolution in (19)F NMR studies of proteins.
A comparison of chemical shift sensitivity of trifluoromethyl tags: optimizing resolution in (19)F NMR studies of proteins.
A comparison of chemical shift sensitivity of trifluoromethyl tags: optimizing resolution in (19)F NMR studies of proteins.
J Biomol NMR. 2015 Mar 27;
Authors: Ye L, Larda ST, Frank Li YF, Manglik A, Prosser RS
Abstract
The elucidation of distinct protein conformers or states by fluorine ((19)F) NMR requires fluorinated moieties whose chemical shifts are most sensitive to subtle changes in the local...
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03-31-2015 07:17 PM
A comparison of chemical shift sensitivity of trifluoromethyl tags: optimizing resolution in 19 F NMR studies of proteins
A comparison of chemical shift sensitivity of trifluoromethyl tags: optimizing resolution in 19 F NMR studies of proteins
Abstract
The elucidation of distinct protein conformers or states by fluorine (19F) NMR requires fluorinated moieties whose chemical shifts are most sensitive to subtle changes in the local dielectric and magnetic shielding environment. In this study we evaluate the effective chemical shift dispersion of a number of thiol-reactive trifluoromethyl probes N-(4-(trifluoromethyl)phenyl)acetamide (BTFMA),...
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03-27-2015 07:43 AM
Enhanced performance large volume dissolution-DNP
From The DNP-NMR Blog:
Enhanced performance large volume dissolution-DNP
Bowen, S. and J.H. Ardenkjaer-Larsen, Enhanced performance large volume dissolution-DNP. J Magn Reson, 2014. 240(0): p. 90-4.
http://www.ncbi.nlm.nih.gov/pubmed/24531395
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05-22-2014 01:48 AM
Hyperpolarization of deuterated metabolites via remote cross-polarization and dissolution dynamic nuclear polarization
From The DNP-NMR Blog:
Hyperpolarization of deuterated metabolites via remote cross-polarization and dissolution dynamic nuclear polarization
Vuichoud, B., et al., Hyperpolarization of deuterated metabolites via remote cross-polarization and dissolution dynamic nuclear polarization. J Phys Chem B, 2014. 118(5): p. 1411-5.
http://www.ncbi.nlm.nih.gov/pubmed/24397585
Optimizing water hyperpolarization and dissolution for sensitivity-enhanced 2D biomolecular NMR
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