Dynamic nuclear polarization exploits electron spin polarization to boost signal-to-noise in magic-angle-spinning (MAS) NMR, creating new opportunities in materials science, structural biology, and metabolomics studies. Since protein NMR spectra recorded under DNP conditions can show improved spectral resolution at 180-200 K compared to 110 K, we investigate the effects of AMUPol and various deuterated TOTAPOL isotopologues on sensitivity and spectral resolution at these temperatures, using proline and reproducibly prepared SH3 domain samples. The TOTAPOL deuteration pattern is optimized for protein DNP MAS NMR, and signal-to-noise per unit time measurements demonstrate the high value of TOTAPOL isotopologues for Protein DNP MAS NMR at 180-200 K. The combined effects of enhancement, depolarization, and proton longitudinal relaxation are surprisingly sample-specific. At 200 K, DNP on SH3 domain standard samples yields a 15-fold increase in signal-to-noise over a sample without radicals. 2D and 3D NCACX/NCOCX spectra were recorded at 200 K within 1 and 13 hours, respectively. Decreasing enhancements with increasing 2H-content at the CH2 sites of the TEMPO rings in CD3-TOTAPOL highlight the importance of protons in a sphere of 4-6 A around the nitroxyl group, presumably for polarization pickup from electron spins.
Rational design of dinitroxide biradicals for efficient cross-effect dynamic nuclear polarization #DNPNMR
From The DNP-NMR Blog:
Rational design of dinitroxide biradicals for efficient cross-effect dynamic nuclear polarization #DNPNMR
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Kubicki, D.J., et al., Rational design of dinitroxide biradicals for efficient cross-effect dynamic nuclear polarization. Chem. Sci., 2016. 7(1): p. 550-558.
http://dx.doi.org/10.1039/C5SC02921J
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01-06-2017 07:43 PM
Rational design of dinitroxide biradicals for efficient cross-effect dynamic nuclear polarization #DNPNMR
From The DNP-NMR Blog:
Rational design of dinitroxide biradicals for efficient cross-effect dynamic nuclear polarization #DNPNMR
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Kubicki, D.J., et al., Rational design of dinitroxide biradicals for efficient cross-effect dynamic nuclear polarization. Chem. Sci., 2016. 7(1): p. 550-558.
http://dx.doi.org/10.1039/C5SC02921J
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12-19-2016 03:37 AM
Correction: Theory of solid effect and cross effect dynamic nuclear polarization with half-integer high-spin metal polarizing agents in rotating solids #DNPNMR
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Correction: Theory of solid effect and cross effect dynamic nuclear polarization with half-integer high-spin metal polarizing agents in rotating solids #DNPNMR
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Corzilius, B., Correction: Theory of solid effect and cross effect dynamic nuclear polarization with half-integer high-spin metal polarizing agents in rotating solids. Phys. Chem. Chem. Phys., 2016. 18(42): p. 29643-29643.
http://dx.doi.org/10.1039/C6CP90249A
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12-17-2016 07:18 AM
Theory of solid effect and cross effect dynamic nuclear polarization with half-integer high-spin metal polarizing agents in rotating solids #DNPNMR
From The DNP-NMR Blog:
Theory of solid effect and cross effect dynamic nuclear polarization with half-integer high-spin metal polarizing agents in rotating solids #DNPNMR
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Corzilius, B., Theory of solid effect and cross effect dynamic nuclear polarization with half-integer high-spin metal polarizing agents in rotating solids. Phys. Chem. Chem. Phys., 2016. 18(39): p. 27190-27204.
http://dx.doi.org/10.1039/C6CP04621E
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11-21-2016 11:02 PM
Phenylazide Hybrid-Silica - Polarization Platform for Dynamic Nuclear Polarization at Cryogenic Temperatures #DNPNMR
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Phenylazide Hybrid-Silica - Polarization Platform for Dynamic Nuclear Polarization at Cryogenic Temperatures #DNPNMR
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Grüning, W.R., et al., Phenylazide Hybrid-Silica - Polarization Platform for Dynamic Nuclear Polarization at Cryogenic Temperatures. Helvetica Chimica Acta, 2016: p. n/a-n/a.
http://dx.doi.org/10.1002/hlca.201600122
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11-19-2016 08:35 PM
The magnetic field dependence of cross-effect dynamic nuclear polarization under magic angle spinning
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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
Fast Passage Dynamic Nuclear Polarization on Rotating Solids
Fast Passage Dynamic Nuclear Polarization on Rotating Solids
Publication year: 2012
Source:Journal of Magnetic Resonance</br>
Frederic Mentink-Vigier, Ümit Akbey, Yonatan Hovav, Shimon Vega, Hartmut Oschkinat, Akiva Feintuch</br>
Magic Angle Spinning (MAS) Dynamic Nuclear Polarization (DNP) has proven to be a very powerful way to improve the signal to noise ratio of NMR experiments on solids. The experiments have in general been interpreted considering the Solid-Effect (SE) and Cross-Effect (CE) DNP mechanisms while ignoring the influence of sample spinning. In this...