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19F Dynamic Nuclear Polarization at Fast Magic Angle Spinning for NMR of HIV-1 Capsid Protein Assemblies.


ABSTRACT: We report remarkably high, up to 100-fold, signal enhancements in 19F dynamic nuclear polarization (DNP) magic angle spinning (MAS) spectra at 14.1 T on HIV-1 capsid protein (CA) assemblies. These enhancements correspond to absolute sensitivity ratios of 12-29 and are of similar magnitude to those seen for 1H signals in the same samples. At MAS frequencies above 20 kHz, it was possible to record 2D 19F-13C HETCOR spectra, which contain long-range intra- and intermolecular correlations. Such correlations provide unique distance restraints, inaccessible in conventional experiments without DNP, for protein structure determination. Furthermore, systematic quantification of the DNP enhancements as a function of biradical concentration, MAS frequency, temperature, and microwave power is reported. Our work establishes the power of DNP-enhanced 19F MAS NMR spectroscopy for structural characterization of HIV-1 CA assemblies, and this approach is anticipated to be applicable to a wide range of large biomolecular systems.

SUBMITTER: Lu M 

PROVIDER: S-EPMC6521953 | biostudies-literature | 2019 Apr

REPOSITORIES: biostudies-literature

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<sup>19</sup>F Dynamic Nuclear Polarization at Fast Magic Angle Spinning for NMR of HIV-1 Capsid Protein Assemblies.

Lu Manman M   Wang Mingzhang M   Sergeyev Ivan V IV   Quinn Caitlin M CM   Struppe Jochem J   Rosay Melanie M   Maas Werner W   Gronenborn Angela M AM   Polenova Tatyana T  

Journal of the American Chemical Society 20190401 14


We report remarkably high, up to 100-fold, signal enhancements in <sup>19</sup>F dynamic nuclear polarization (DNP) magic angle spinning (MAS) spectra at 14.1 T on HIV-1 capsid protein (CA) assemblies. These enhancements correspond to absolute sensitivity ratios of 12-29 and are of similar magnitude to those seen for <sup>1</sup>H signals in the same samples. At MAS frequencies above 20 kHz, it was possible to record 2D <sup>19</sup>F-<sup>13</sup>C HETCOR spectra, which contain long-range intra  ...[more]

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