Journal
JOURNAL OF MATERIALS CHEMISTRY B
Volume 8, Issue 31, Pages 6827-6836Publisher
ROYAL SOC CHEMISTRY
DOI: 10.1039/d0tb00614a
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Funding
- Newton International Fellowship Alumni Follow on Funding of the Royal Society [AL\180018]
- EPSRC
- BBSRC [PR140003]
- University of Warwick from the Birmingham Science City Advanced Materials Projects 1 and 2 - Advantage West Midlands (AWM)
- European Regional Development Fund (ERDF)
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Amorphous drug-polymer formulations are complex materials and often challenging to characterize, even more so if the small molecule component itself is increasingly complex. In this work, we present N-14-H-1 HMQC magic-angle spinning (MAS) NMR experiments in the solid state as a promising tool to study amorphous formulations. Poly(2-oxazoline) based polymer micelles loaded with different amounts of the cancer drug paclitaxel serve to highlight the possibilities offered by these experiments: while the dense core of these polymeric micelles prevents NMR spectroscopic analysis in solution and the very similar N-15 chemical shifts hamper a solid-state NMR characterization based on this nucleus, N-14 is a very versatile alternative. N-14-H-1 HMQC experiments yield well-separated signals, which are spread over a large ppm range, and provide information on the symmetry of the nitrogen environment and probe N-14-H-1 through-space proximities. In this way, the overall complexity can be narrowed down to specific N-containing environments. The results from the experiments presented here represent a valuable puzzle piece, which helps to improve the structural understanding of drug-polymer formulations. It can be straightforwardly combined with complementary NMR spectroscopic experiments and other analytical techniques.
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