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  • Title: 19 F Magic Angle Spinning Dynamic Nuclear Polarization Enhanced NMR Spectroscopy.
    Author: Viger-Gravel J, Avalos CE, Kubicki DJ, Gajan D, Lelli M, Ouari O, Lesage A, Emsley L.
    Journal: Angew Chem Int Ed Engl; 2019 May 27; 58(22):7249-7253. PubMed ID: 30945400.
    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 19 F 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 19 F DNP enhancements of over 100 at 9.4 T. We applied this protocol to obtain DNP-enhanced 19 F and 19 F-13 C 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 19 F MAS spectra from fluorinated materials.
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