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Trehalose matrices for high temperature dynamic nuclear polarization enhanced solid state NMR.

Monu Kaushik1, Hugo Lingua2, Gabriele Stevanato3

  • 1Centre de RMN à Très Hauts Champs, Université de Lyon/CNRS/ENS Lyon/UCB Lyon 1, 5 Rue de la Doua, 69100 Villeurbanne, France. anne.lesage@ens-lyon.fr.

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New trehalose-based matrices significantly enhance dynamic nuclear polarization (DNP) for solid-state NMR spectroscopy. These matrices perform well at higher temperatures, overcoming limitations of traditional formulations for improved sensitivity.

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Area of Science:

  • Solid-state NMR spectroscopy
  • Dynamic Nuclear Polarization (DNP)

Background:

  • Dynamic nuclear polarization (DNP) enhances solid-state NMR sensitivity at cryogenic temperatures.
  • Conventional polarizing agents like AMUPol and TEKPol show reduced performance at elevated temperatures.
  • Existing sample formulations are optimized for low-temperature DNP experiments.

Purpose of the Study:

  • To develop novel trehalose-based DNP polarizing matrices for biomolecular assemblies.
  • To investigate the DNP efficiency of these new matrices with various polarizing agents and formulations.
  • To evaluate the performance of trehalose matrices at temperatures above 150 K.

Main Methods:

  • Formulation of trehalose-based DNP polarizing matrices.
  • Screening DNP efficiency based on radical concentration, hydration, and protein content.
  • Comparison of trehalose matrices with conventional water/glycerol mixtures at various temperatures.

Main Results:

  • Trehalose matrices demonstrate sizeable DNP enhancement factors at 100 K and 9.4 T.
  • New polarizing media, including a tethered biradical, show promising DNP efficiency.
  • Trehalose matrices outperform water/glycerol mixtures at temperatures above 180 K.

Conclusions:

  • Trehalose matrices are a viable DNP medium for temperatures exceeding 150 K.
  • These matrices overcome limitations of conventional formulations that soften at higher temperatures.
  • Opens new possibilities for DNP-enhanced solid-state NMR near ambient temperatures.