Dynamic Nuclear Polarization of Sedimented Solutes
Author(s)
Ravera, Enrico; Michaelis, Vladimir K.; Rosa, Camilla; Luchinat, Claudio; Bertini, Ivano; Griffin, Robert Guy; Corzilius, Bjorn; ... Show more Show less
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Using the 480 kDa iron-storage protein complex, apoferritin (ApoF), as an example, we demonstrate that sizable dynamic nuclear polarization (DNP) enhancements can be obtained on sedimented protein samples. In sedimented solute DNP (SedDNP), the biradical polarizing agent is co-sedimented with the protein, but in the absence of a glass-forming agent. We observe DNP enhancement factors ε > 40 at a magnetic field of 5 T and temperatures below 90 K, indicating that the protein sediment state is “glassy” and suitable to disperse the biradical polarizing agent upon freezing. In contrast, frozen aqueous solutions of ApoF yield ε ≈ 2. Results of SedDNP are compared to those obtained from samples prepared using the traditional glass-forming agent glycerol. Collectively, these and results from previous investigations suggest that the sedimented state can be functionally described as a “microcrystalline glass” and in addition provide a new approach for preparation of samples for DNP experiments.
Date issued
2013-01Department
Massachusetts Institute of Technology. Department of Chemistry; Francis Bitter Magnet Laboratory (Massachusetts Institute of Technology)Journal
Journal of the American Chemical Society
Publisher
American Chemical Society (ACS)
Citation
Ravera, Enrico, Björn Corzilius, Vladimir K. Michaelis, Camilla Rosa, Robert G. Griffin, Claudio Luchinat, and Ivano Bertini. “Dynamic Nuclear Polarization of Sedimented Solutes.” Journal of the American Chemical Society 135, no. 5 (February 6, 2013): 1641–1644.
Version: Author's final manuscript
ISSN
0002-7863
1520-5126