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

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

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.

Publication types

  • Research Support, Non-U.S. Gov't
  • Research Support, N.I.H., Extramural

MeSH terms

  • Electron Spin Resonance Spectroscopy* / methods
  • Membrane Proteins / chemistry
  • Microscopy, Atomic Force
  • Microscopy, Electron
  • Nuclear Magnetic Resonance, Biomolecular* / methods
  • Peptides / chemistry
  • Protein Aggregates
  • Proteins / chemistry
  • Proteins / isolation & purification
  • Proteins / ultrastructure
  • Ultracentrifugation* / instrumentation
  • Ultracentrifugation* / methods

Substances

  • Membrane Proteins
  • Peptides
  • Protein Aggregates
  • Proteins