19F Magic Angle Spinning Dynamic Nuclear Polarization Enhanced NMR Spectroscopy

Jasmine Viger-Gravel, Claudia E. Avalos, Dominik J. Kubicki, David Gajan, Moreno Lelli, Olivier Ouari, Anne Lesage, Lyndon Emsley

Research output: Contribution to journalArticlepeer-review

Abstract

The introduction of high-frequency, high-power microwave sources, tailored biradicals, and low-temperature magic angle spinning (MAS) probes has led to a rapid development of hyperpolarization strategies for solids and frozen solutions, leading to large gains in NMR sensitivity. Here, we introduce a protocol for efficient hyperpolarization of 19F nuclei in MAS DNP enhanced NMR spectroscopy. We identified trifluoroethanol-d3 as a versatile glassy matrix and show that 12 mm AMUPol (with microcrystalline KBr) provides direct 19F DNP enhancements of over 100 at 9.4 T. We applied this protocol to obtain DNP-enhanced 19F and 19F–13C cross-polarization (CP) spectra for an active pharmaceutical ingredient and a fluorinated mesostructured hybrid material, using incipient wetness impregnation, with enhancements of approximately 25 and 10 in the bulk solid, respectively. This strategy is a general and straightforward method for obtaining enhanced 19F MAS spectra from fluorinated materials.

Original languageEnglish (US)
Pages (from-to)7249-7253
Number of pages5
JournalAngewandte Chemie - International Edition
Volume58
Issue number22
DOIs
StatePublished - May 27 2019

Keywords

  • active pharmaceutical ingredients
  • dynamic nuclear polarization
  • magic angle spinning
  • NMR spectroscopy

ASJC Scopus subject areas

  • Catalysis
  • Chemistry(all)

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