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Core-Shell Structure of Organic Crystalline Nanoparticles Determined by Relayed Dynamic Nuclear Polarization NMR.
Journal of Physical Chemistry. A 2018 November 9
The structure of crystalline nanoparticles (CNPs) is determined using dynamic nuclear polarization (DNP) enhanced NMR spectroscopy experiments. The CNPs are composed of a crystalline core containing an active pharmaceutical ingredient (compound P), coated with a layer of PEG (DSPE-PEG 5000) located at the crystal surface, in a D2 O suspension. Relayed DNP experiments are performed to study 1 H-1 H spin diffusion and to determine the size of the crystalline core as well as the thickness of the PEG overlayer. This is achieved through selective doping to create a heterogeneous system in which the D2 O contains glycerol and organic radicals, which act as polarization sources, and the CNPs are exempt of radical molecules. We observe features that are characteristic of a core-shell system: high and constant DNP enhancement for components located in the surrounding radical solution, short build-up times for the PEG layer, and longer build-up times and time dependent enhancements for compound P. By comparing numerical simulations and experimental data, we propose a structural model for the CNPs with a core-shell organization and a high affinity between the radical and the PEG molecules.
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