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J Biomol NMR. 2017 Mar;67(3):165-178. doi: 10.1007/s10858-017-0089-6. Epub 2017 Feb 22.

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

Author information

1
Department of Structural Biology, University of Pittsburgh School of Medicine, Pittsburgh, PA, 15260, USA.
2
Department of Cell Biology, University of Pittsburgh School of Medicine, Pittsburgh, Pennsylvania, 15260, USA.
3
Department of Structural Biology, University of Pittsburgh School of Medicine, Pittsburgh, PA, 15260, USA. vanderwel@pitt.edu.

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.

KEYWORDS:

Hydration; MAS NMR; Sample packing; Sedimentation; Ultracentrifugation

PMID:
28229262
PMCID:
PMC5445385
DOI:
10.1007/s10858-017-0089-6
[Indexed for MEDLINE]
Free PMC Article

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