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3D-Printable centrifugal devices for biomolecular solid state NMR rotors.

Thomas M Osborn Popp1, Brandon T Matchett1, Rashawn G Green1

  • 1Department of Chemistry and Chemical Biology, Rutgers, The State University of New, Jersey, Piscataway, NJ 08854, United States.

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Summary

New 3D-printed devices enable efficient packing of biomolecular samples into small rotors for high-speed magic angle spinning (MAS) solid-state NMR, improving spectral resolution.

Keywords:
3D printingBiomolecular solidsCentrifugal packing deviceFast-MASMagic angle spinningSolid state NMR

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Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy
  • Biomolecular structure determination
  • Materials science and engineering

Background:

  • High magic angle spinning (MAS) rates (>100 kHz) enhance resolution in 1H-detected solid-state NMR for biomolecules.
  • Sample preparation, particularly packing rotors, presents challenges due to biomolecular sample properties and small rotor dimensions.

Purpose of the Study:

  • To design and validate 3D-printable centrifugal devices for efficient and consistent packing of biomolecular samples into 0.7 mm rotors.
  • To address challenges in preparing samples for high-speed MAS solid-state NMR experiments.
  • To provide accessible tools for the solid-state NMR community.

Main Methods:

  • Design and fabrication of 3D-printable centrifugal packing devices.
  • Utilizing crystalline protein slurries and viscous phospholipid samples.
  • Demonstration using 1H-detected solid-state NMR at 105 kHz MAS rates.

Main Results:

  • Successful design and implementation of centrifugal packing devices for 0.7 mm rotors.
  • Demonstrated efficient and consistent packing of biomolecular samples.
  • Developed devices for various rotor sizes and styles, confirming efficacy at 105 kHz MAS.

Conclusions:

  • 3D-printable centrifugal devices significantly improve biomolecular sample packing for high-speed MAS solid-state NMR.
  • Openly accessible designs promote community collaboration and further development.
  • These tools facilitate higher resolution biomolecular solid-state NMR studies.