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Nowak, Maciej, Dyba, Aleksandra J., Gołkowska, Anna M., Nieckarz, Aleksandra, Krajewska, Karolina, Malec, Katarzyna, Iuga, Dinu, Karolewicz, Bożena, Khimyak, Yaroslav Z. 
ORCID: https://orcid.org/0000-0003-0424-4128 and Nartowski, Karol P.
(2023)
Probing fluconazole deposition inside mesoporous silica using solid-state NMR spectroscopy: crystallization of a confined metastable form and phase transformations under storage conditions.
International Journal of Pharmaceutics, 645.
ISSN 0378-5173
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Abstract
Encapsulation of molecules into mesoporous silica carriers continues to attract considerable interest in the area of drug delivery and crystal engineering. Here, MCM-41, SBA-15 and MCF silica matrices were used to encapsulate fluconazole (FLU), a pharmaceutically relevant molecule with known conformational flexibility, using the melting method. The composites have been characterized using 1H, 13C and 19F NMR spectroscopy, nitrogen adsorption, PXRD and thermal analysis (DSC, TGA). Drug loading up to 50 wt% allowed us to probe the crystallization process and to detect different local environments of confined FLU molecules. 19F NMR spectroscopy enabled us to detect the gradual pore filling of silica with FLU and differentiate the amorphous domains and surface species. The use of the complementary structural and thermal techniques enabled us to monitor crystallization of the metastable FLU form II in MCF. Using 1H and 19F NMR spectroscopy we observed pore-size dependent reversible dehydration/hydration behaviour in the MCM and SBA composites. As water content has considerable importance in understanding of physicochemical stability and shelf-life of pharmaceutical formulations, experimental evidence of the effect of API-water-carrier interactions on the API adsorption mechanism on silica surface is highlighted.
| Item Type: | Article |
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| Additional Information: | Funding Information: The authors would like to thank the Laboratory of Elemental Analysis and Structural Research at the Faculty of Pharmacy at the Wroclaw Medical University for the access to PXRD, DSC, and TGA instruments. A.J.D. and A.M.G. thank the National Science Centre in Poland for a postgraduate scholarship via a MOZART grant (UMO-2020/01/Y/ST4/00101). K.P.N. and A.M.G. are grateful for the access to the University of East Anglia NMR platforms as part of UEA Faculty of Science facilities. The access to The UK High-Field Solid-State NMR Facility (University of Warwick) had financial support from the PANACEA project that has received funding from the European Union's Horizon 2020 research and innovation programme under Grant Agreement No 101008500. This research was funded by the Ministry of Science and Higher Education in Poland via grant number SUBK.D190.22.005. |
| Uncontrolled Keywords: | pharmaceutical science ,/dk/atira/pure/subjectarea/asjc/3000/3003 |
| Faculty \ School: | Faculty of Science > School of Pharmacy Faculty of Science |
| UEA Research Groups: | Faculty of Science > Research Groups > Pharmaceutical Materials and Soft Matter |
| Related URLs: | |
| Depositing User: | LivePure Connector |
| Date Deposited: | 19 Sep 2023 11:30 |
| Last Modified: | 07 Oct 2023 01:22 |
| URI: | https://ueaeprints.uea.ac.uk/id/eprint/93063 |
| DOI: | 10.1016/j.ijpharm.2023.123403 |
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