Dynamic nuclear polarization has been developed to overcome the limitations of the inherently low signal intensity of NMR spectroscopy. This technique promises to be particularly useful for solid-state NMR spectroscopy where the signals are broadened over a larger frequency range and most investigations rely on recording low gamma nuclei. To extend the range of possible investigations, a triple-resonance flat-coil solid-state NMR probe is presented with microwave irradiation capacities allowing the investigation of static samples at temperatures of 100 K, including supported lipid bilayers. The probe performance allows for two-dimensional separated local field experiments with high-power Lee-Goldberg decoupling and cross-polarization under simultaneous irradiation from a gyrotron microwave generator. Efficient cooling of the sample turned out to be essential for best enhancements and line shape and necessitated the development of a dedicated cooling chamber. Furthermore, a new membrane-anchored biradical is presented, and the geometry of supported membranes was optimized not only for good membrane alignment, handling, stability, and filling factor of the coil but also for heat and microwave dissipation. Enhancement factors of 17-fold were obtained, and a two-dimensional PISEMA spectrum of a transmembrane helical peptide was obtained in less than 2 h.
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High-Field Solid-State NMR with Dynamic Nuclear Polarization #DNPNMR
From The DNP-NMR Blog:
High-Field Solid-State NMR with Dynamic Nuclear Polarization #DNPNMR
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Lee, D., S. Hediger, and G.D. Paëpe, High-Field Solid-State NMR with Dynamic Nuclear Polarization, in Modern Magnetic Resonance, G.A. Webb, Editor. 2017, Springer International Publishing: Cham. p. 1-17.
https://doi.org/10.1007/978-3-319-28275-6_73-1
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01-08-2018 03:44 PM
Dynamic Nuclear Polarization/Solid-State NMR Spectroscopy of Membrane Polypeptides: Free-Radical Optimization for Matrix-Free Lipid Bilayer Samples #DNPNMR
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Dynamic Nuclear Polarization/Solid-State NMR Spectroscopy of Membrane Polypeptides: Free-Radical Optimization for Matrix-Free Lipid Bilayer Samples #DNPNMR
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Salnikov, E.S., et al., Dynamic Nuclear Polarization/Solid-State NMR Spectroscopy of Membrane Polypeptides: Free-Radical Optimization for Matrix-Free Lipid Bilayer Samples. ChemPhysChem, 2017. 18(15): p. 2103-2113.
https://www.ncbi.nlm.nih.gov/pubmed/28574169
Characterizing Substrate-Surface Interactions on Alumina-Supported Metal Catalysts by Dynamic Nuclear Polarization-Enhanced Double-Resonance NMR Spectroscopy #DNPNMR
From The DNP-NMR Blog:
Characterizing Substrate-Surface Interactions on Alumina-Supported Metal Catalysts by Dynamic Nuclear Polarization-Enhanced Double-Resonance NMR Spectroscopy #DNPNMR
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Perras, F.A., et al., Characterizing Substrate-Surface Interactions on Alumina-Supported Metal Catalysts by Dynamic Nuclear Polarization-Enhanced Double-Resonance NMR Spectroscopy. J Am Chem Soc, 2017. 139(7): p. 2702-2709.
https://www.ncbi.nlm.nih.gov/pubmed/28112506
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06-13-2017 06:55 AM
[NMR paper] Dynamic nuclear polarization / solid-state NMR of membrane polypeptides. Free radical optimization for matrix-free lipid bilayer samples.
Dynamic nuclear polarization / solid-state NMR of membrane polypeptides. Free radical optimization for matrix-free lipid bilayer samples.
Related Articles Dynamic nuclear polarization / solid-state NMR of membrane polypeptides. Free radical optimization for matrix-free lipid bilayer samples.
Chemphyschem. 2017 Jun 02;:
Authors: Ouari O, Salnikov ES, Abel S, Karthikeyan G, Karoui H, Aussenac F, Tordo P, Bechinger B
Abstract
Dynamic Nuclear Polarization boosts the sensitivity of NMR spectroscopy by orders of magnitude making...
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06-03-2017 11:49 AM
Solid-State NMR/Dynamic Nuclear Polarization of Polypeptides in Planar Supported Lipid Bilayers
From The DNP-NMR Blog:
Solid-State NMR/Dynamic Nuclear Polarization of Polypeptides in Planar Supported Lipid Bilayers
Salnikov, E.S., et al., Solid-State NMR/Dynamic Nuclear Polarization of Polypeptides in Planar Supported Lipid Bilayers. J Phys Chem B, 2015. 119(46): p. 14574-83.
http://www.ncbi.nlm.nih.gov/pubmed/26487390
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03-02-2016 07:20 PM
[NMR paper] Optimizing oriented planar-supported lipid samples for solid-state protein NMR.
Optimizing oriented planar-supported lipid samples for solid-state protein NMR.
Related Articles Optimizing oriented planar-supported lipid samples for solid-state protein NMR.
Biophys J. 2005 Oct;89(4):2792-805
Authors: Rainey JK, Sykes BD
Sample orientation relative to the static magnetic field of an NMR spectrometer allows study of membrane proteins in the lipid bilayer setting. The straightforward preparation and handling of extremely thin mica substrates with consistent surface properties has prompted us to examine oriented phospholipid...
Solid-State NMR/Dynamic Nuclear Polarization of Polypeptides in Planar Supported Lipid Bilayers #DNPNMR #NMR
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