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On the use of ultracentrifugal devices for routine sample preparation in biomolecular magic-angle-spinning NMR

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Abstract

A number of recent advances in the field of magic-angle-spinning (MAS) solid-state NMR have enabled its application to a range of biological systems of ever increasing complexity. To retain biological relevance, these samples are increasingly studied in a hydrated state. At the same time, experimental feasibility requires the sample preparation process to attain a high sample concentration within the final MAS rotor. We discuss these considerations, and how they have led to a number of different approaches to MAS NMR sample preparation. We describe our experience of how custom-made (or commercially available) ultracentrifugal devices can facilitate a simple, fast and reliable sample preparation process. A number of groups have since adopted such tools, in some cases to prepare samples for sedimentation-style MAS NMR experiments. Here we argue for a more widespread adoption of their use for routine MAS NMR sample preparation.

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Fig. 1
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[Adapted from (Mandal et al. 2015), Copyright 2015, with permission from Elsevier.] c TEM on [U–13C–15N]-labeled huntingtin exon 1 fibrils prepared for ssNMR. d 13C–13C CP DARR spectrum of 4.4 mg of htt exon1 fibrils measured at 275 K and 13 kHz MAS. Panels c–d are adapted from (Hoop et al. 2016). e AFM on C18–(PEPAu M−ox)2 fibers. f 13C–13C CP DARR spectrum of 1.9 mg of C18–(PEPAu M−ox)2 peptide nanofibrils measured at 277 K. Panels e–f are adapted with permission from (Merg et al. 2016). Copyright 2016 American Chemical Society. The NMR measurements were performed on 800 and 600 MHz (1H) spectrometer using 3.2 mm MAS rotors

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Acknowledgements

We thank Mike Delk for his help with the NMR experiments. Funding support was from the University of Pittsburgh and the National Institutes of Health grants R01GM112678 and R01GM113908 (P.v.d.W.), and T32 GM088119 (J.C.B.).

Author contributions

TW and PvdW designed the packing tool. TW fabricated the packing tool. AM prepared samples. AM packed samples. AM and JCB performed MAS NMR experiments. JCB performed transmission electron microscopy measurements. AM and PvdW wrote the manuscript. All authors have read and edited the manuscript.

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Authors and Affiliations

  1. Department of Structural Biology, University of Pittsburgh School of Medicine, Pittsburgh, PA, 15260, USA

    Abhishek Mandal, Jennifer C. Boatz & Patrick C. A. van der Wel

  2. Department of Cell Biology, University of Pittsburgh School of Medicine, Pittsburgh, Pennsylvania, 15260, USA

    Travis B. Wheeler

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  1. Abhishek Mandal
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  2. Jennifer C. Boatz
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  3. Travis B. Wheeler
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  4. Patrick C. A. van der Wel
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Correspondence to Patrick C. A. van der Wel.

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Mandal, A., Boatz, J.C., Wheeler, T.B. et al. On the use of ultracentrifugal devices for routine sample preparation in biomolecular magic-angle-spinning NMR. J Biomol NMR 67, 165–178 (2017). https://doi.org/10.1007/s10858-017-0089-6

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  • DOI: https://doi.org/10.1007/s10858-017-0089-6

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