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Strategies for Efficient Sample Preparation for Dynamic Nuclear Polarization Solid-State NMR of Biological Macromolecules

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Protein NMR

Part of the book series: Methods in Molecular Biology ((MIMB,volume 1688))

Abstract

Solid-state NMR (SSNMR) is a powerful tool for the elucidation of structure and dynamics in biological macromolecules. Over the years, SSNMR spectroscopists have developed an array of techniques enabling the measurement of internuclear correlations, distances, and torsional angles; these have been applied to the study of a number of biological systems that are difficult to study by X-ray crystallography and solution NMR, including key biological targets such as membrane proteins and amyloid fibrils. Applications of SSNMR to other topic areas, including materials science, pharmaceuticals, and small molecules, have also flourished in recent years. These studies, however, have always been hampered by the low inherent sensitivity of SSNMR, requiring large amounts of both sample and time for data collection. By taking advantage of unpaired electrons doped into a sample as a ready source of additional nuclear polarization, dynamic nuclear polarization (DNP) has brought about large improvements in SSNMR sensitivity. These, in turn, have enabled structural studies of previously inaccessible targets, such as large protein complexes, nucleic acids, viral capsids, and membrane proteins in vivo. Herein, we focus on sample preparation strategies and considerations for scientists interested in applying DNP to challenging systems.

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Acknowledgment

The authors would like to thank Dr. James Kempf, Dr. Shane Pawsey, Bryce Smith, and Christopher Hickey of Bruker Biospin for many helpful discussions, figures, and photographs.

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Authors and Affiliations

  1. New York Structural Biology Center, 89 Convent Avenue, New York, NY, 10027, USA

    Boris Itin

  2. Bruker Biospin Corporation, 15 Fortune Drive, Billerica, MA, 01821, USA

    Ivan V. Sergeyev

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  1. Boris Itin
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  2. Ivan V. Sergeyev
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Correspondence to Boris Itin .

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Editors and Affiliations

  1. Department of Chemistry and Biochemistry, The City College of New York, New York, New York, USA

    Ranajeet Ghose

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Itin, B., Sergeyev, I.V. (2018). Strategies for Efficient Sample Preparation for Dynamic Nuclear Polarization Solid-State NMR of Biological Macromolecules. In: Ghose, R. (eds) Protein NMR. Methods in Molecular Biology, vol 1688. Humana Press, New York, NY. https://doi.org/10.1007/978-1-4939-7386-6_7

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  • DOI: https://doi.org/10.1007/978-1-4939-7386-6_7

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  • Publisher Name: Humana Press, New York, NY

  • Print ISBN: 978-1-4939-7385-9

  • Online ISBN: 978-1-4939-7386-6

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