Preprints
https://doi.org/10.5194/mr-2021-13
https://doi.org/10.5194/mr-2021-13

  04 Feb 2021

04 Feb 2021

Review status: this preprint is currently under review for the journal MR.

Competing Transfer Pathways in Direct and Indirect Dynamic Nuclear Polarization MAS NMR Experiments on HIV-1 Capsid Assemblies: Implications for Sensitivity and Resolution

Ivan V. Sergeyev1, Caitlin M. Quinn2, Jochem Struppe1, Angela Gronenborn3,4, and Tatyana Polenova2,3 Ivan V. Sergeyev et al.
  • 1Bruker Biospin Corporation, 15 Fortune Drive, Billerica, Massachusetts 01821, United States
  • 2Department of Chemistry and Biochemistry, University of Delaware, Newark, Delaware 19716, United States
  • 3Pittsburgh Center for HIV Protein Interactions, University of Pittsburgh School of Medicine, 1051 Biomedical Science Tower 3, 3501 Fifth Avenue, Pittsburgh, Pennsylvania 15261, United States
  • 4Department of Structural Biology, University of Pittsburgh School of Medicine, 3501 Fifth Ave., Pittsburgh, PA 15261, United States

Abstract. Dynamic nuclear polarization-enhanced (DNP) magic angle spinning (MAS) NMR of biological systems is a rapidly growing field. Large signal enhancements make the technique particularly attractive for signal-limited cases, such as studies of complex biological assemblies or at natural isotopic abundance. However, spectral resolution is considerably reduced compared to ambient-temperature non-DNP spectra. Herein, we report a systematic investigation into sensitivity and resolution of 1D and 2D 13C-detected DNP MAS NMR experiments on HIV-1 CA tubular assemblies. We show that the magnitude and sign of signal enhancement as well as the homogeneous line width are strongly dependent on the biradical concentration, the dominant polarization transfer pathway, and the enhancement buildup time. Our findings provide guidance for optimal choice of sample preparation and experimental conditions in DNP experiments.

Ivan V. Sergeyev et al.

Status: open (until 04 Mar 2021)

Comment types: AC – author | RC – referee | CC – community | EC – editor | CEC – chief editor | : Report abuse
  • RC1: 'Comment on mr-2021-13', Anja Böckmann, 05 Feb 2021 reply
  • RC2: 'Comment on mr-2021-13', Björn Corzilius, 23 Feb 2021 reply

Ivan V. Sergeyev et al.

Ivan V. Sergeyev et al.

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Short summary
Dynamic nuclear polarization (DNP) magic angle spinning NMR yields huge signal enhancements and is attractive for signal-limited cases. We studied polarization transfer pathways underlying sensitivity and resolution in DNP experiments on tubular assemblies of HIV-1 CA protein. All three polarization transfer pathways are simultaneously active and can be selected by carefully choosing experimental conditions. Our study highlights the unique capabilities of DNP for structural biology applications.