Perras, F.A., T. Kobayashi, and M. Pruski, Magnetic resonance imaging of DNP enhancements in a rotor spinning at the magic angle. J Magn Reson, 2016. 264: p. 125-30.
Simulations performed on model, static, samples have shown that the microwave power is non-uniformly distributed in the magic angle spinning (MAS) rotor when using conventional dynamic nuclear polarization (DNP) instrumentation. Here, we applied the stray-field magic angle spinning imaging (STRAFI-MAS) experiment to generate a spatial map of the DNP enhancements in a full rotor, which is spun at a low rate in a commercial DNP-MAS NMR system. Notably, we observed that the enhancement factors produced in the center of the rotor can be twice as large as those produced at the top of the rotor. Surprisingly, we observed that the largest enhancement factors are observed along the axis of the rotor as opposed to against its walls, which are most directly irradiated by the microwave beam. We lastly observed that the distribution of enhancement factors can be moderately improved by degassing the sample and increasing the microwave power. The inclusion of dielectric particles greatly amplifies the enhancement factors throughout the rotor. The STRAFI-MAS approach can provide useful guidance for optimizing the access of microwave power to the sample, and thereby lead to further increases in sensitivity of DNP-MAS NMR.
The magnetic field dependence of cross-effect dynamic nuclear polarization under magic angle spinning
From The DNP-NMR Blog:
The magnetic field dependence of cross-effect dynamic nuclear polarization under magic angle spinning
Mance, D., et al., The magnetic field dependence of cross-effect dynamic nuclear polarization under magic angle spinning. J. Chem. Phys., 2015. 142(23): p. 234201.
doi:http://dx.doi.org/10.1063/1.4922219
nmrlearner
News from NMR blogs
0
07-06-2015 04:35 PM
[NMR paper] Quadruple-Resonance Magic-Angle Spinning NMR Spectroscopy of Deuterated Solid Proteins.
Quadruple-Resonance Magic-Angle Spinning NMR Spectroscopy of Deuterated Solid Proteins.
Related Articles Quadruple-Resonance Magic-Angle Spinning NMR Spectroscopy of Deuterated Solid Proteins.
Angew Chem Int Ed Engl. 2014 Jan 29;
Authors: Akbey U, Nieuwkoop AJ, Wegner S, Voreck A, Kunert B, Bandara P, Engelke F, Nielsen NC, Oschkinat H
Abstract
(1) H-detected magic-angle spinning NMR experiments facilitate structural biology of solid proteins, which requires using deuterated proteins. However, often amide protons cannot be back-exchanged...
nmrlearner
Journal club
0
01-30-2014 05:38 PM
[NMR paper] Magic angle spinning nuclear magnetic resonance spectroscopy of g protein-coupled receptors.
Magic angle spinning nuclear magnetic resonance spectroscopy of g protein-coupled receptors.
Related Articles Magic angle spinning nuclear magnetic resonance spectroscopy of g protein-coupled receptors.
Methods Enzymol. 2013;522:365-89
Authors: Goncalves J, Eilers M, South K, Opefi CA, Laissue P, Reeves PJ, Smith SO
Abstract
G protein-coupled receptors (GPCRs) represent the largest family of membrane receptors and mediate a diversity of cellular processes. These receptors have a common seven-transmembrane helix structure, yet have evolved...
nmrlearner
Journal club
0
02-05-2013 09:51 PM
Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25K
Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25K
January 2013
Publication year: 2013
Source:Journal of Magnetic Resonance, Volume 226</br>
</br>
We describe an apparatus for solid state nuclear magnetic resonance (NMR) with dynamic nuclear polarization (DNP) and magic-angle spinning (MAS) at 20–25K and 9.4Tesla. The MAS NMR probe uses helium to cool the sample space and nitrogen gas for MAS drive and bearings, as described earlier , but also includes a corrugated waveguide for transmission of microwaves from...
nmrlearner
Journal club
0
12-15-2012 09:51 AM
Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25 K
Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25 K
Available online 20 November 2012
Publication year: 2012
Source:Journal of Magnetic Resonance</br>
</br>
We describe an apparatus for solid state nuclear magnetic resonance (NMR) with dynamic nuclear polarization (DNP) and magic-angle spinning (MAS) at 20-25 K and 9.4 Tesla. The MAS NMR probe uses helium to cool the sample space and nitrogen gas for MAS drive and bearings, as described earlier (Thurber et al., J. Magn. Reson. 2008) , but also includes a...
nmrlearner
Journal club
0
12-01-2012 06:10 PM
Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25 K
Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25 K
Publication year: 2012
Source:Journal of Magnetic Resonance</br>
Kent R. Thurber, Alexey Potapov, Wai-Ming Yau, Robert Tycko</br>
We describe an apparatus for solid state nuclear magnetic resonance (NMR) with dynamic nuclear polarization (DNP) and magic-angle spinning (MAS) at 20-25 K and 9.4 Tesla. The MAS NMR probe uses helium to cool the sample space and nitrogen gas for MAS drive and bearings, as described earlier (Thurber et al., J. Magn. Reson. 2008) ,...
nmrlearner
Journal club
0
11-21-2012 04:33 AM
Automated protein resonance assignments of magic angle spinning solid-state NMR spect
Automated protein resonance assignments of magic angle spinning solid-state NMR spectra of β1 immunoglobulin binding domain of protein G (GB1)
Abstract Magic-angle spinning solid-state NMR (MAS SSNMR) represents a fast developing experimental technique with great potential to provide structural and dynamics information for proteins not amenable to other methods. However, few automated analysis tools are currently available for MAS SSNMR. We present a methodology for automating protein resonance assignments of MAS SSNMR spectral data and its application to experimental peak lists of the...
nmrlearner
Journal club
0
10-15-2010 05:16 PM
Automated protein resonance assignments of magic angle spinning solid-state NMR spect
Automated protein resonance assignments of magic angle spinning solid-state NMR spectra of ?1 immunoglobulin binding domain of protein G (GB1).
Related Articles Automated protein resonance assignments of magic angle spinning solid-state NMR spectra of ?1 immunoglobulin binding domain of protein G (GB1).
J Biomol NMR. 2010 Oct 8;
Authors: Moseley HN, Sperling LJ, Rienstra CM
Magic-angle spinning solid-state NMR (MAS SSNMR) represents a fast developing experimental technique with great potential to provide structural and dynamics information for...