14N-1H HMQC solid-state NMR as a powerful tool to study amorphous formulations – an exemplary study of paclitaxel loaded polymer micelles
| Autor: | Steven P. Brown, Dinu Iuga, Robert Luxenhofer, Marvin Grüne, Ann-Christin Pöppler |
|---|---|
| Jazyk: | angličtina |
| Rok vydání: | 2020 |
| Předmět: |
chemistry.chemical_classification
Materials science Chemical shift Biomedical Engineering Solid-state Nanotechnology General Chemistry General Medicine Nuclear magnetic resonance spectroscopy Polymer Small molecule Micelle Characterization (materials science) Amorphous solid chemistry.chemical_compound chemistry Solid-state nuclear magnetic resonance Paclitaxel Chemical engineering TheoryofComputation_ANALYSISOFALGORITHMSANDPROBLEMCOMPLEXITY Yield (chemistry) General Materials Science QC RC |
| ISSN: | 2050-750X |
| Popis: | 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 14N-1H 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 an NMR spectroscopic analysis in solution and the very similar 15N chemical shifts hamper a solid-state NMR characterization based on this nucleus, 14N is a very versatile alternative. 14N-1H HMQC experiments yield well-separated signals, which are spread over a large ppm range, provide information on the symmetry of the nitrogen environment and probe 14N-1H 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.\ud \ud |
| Databáze: | OpenAIRE |
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