Evidence of a New Crystalline Phase of Prednisolone Obtained from the Study of the Hydration–Dehydration Mechanisms of the Sesquihydrate
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials
2.2. TGA-DSC-MS
2.3. XRPD and Temperature Resolved XRPD
2.4. Thermal Microscopy
2.5. Dynamic Vapor Sorption
2.6. Molecular Modeling
3. Results and Discussion
3.1. Thermal Behavior of Prednisolone Sesquihydrate during Dehydration
3.2. Hydration/Dehydration Behavior versus Relative Humidity of Prednisolone
- (1)
- There is a slight compensation of some degrees of vacancy for O13 by a higher Beq. Consistently, several TGA analyses tend to converge to 1.3 equivalents of water molecules starting from a sample conditioned at room temperature and under an ambient atmosphere. This could therefore indicate the non-stoichiometric behavior of the sesquihydrate. The maximum stoichiometry (1.5 water molecules) is reached only with high RH (cf. DVS data).
- (2)
- The three water molecules O12-O13-O11 form a cluster, as shown in Figure 11. The slight global deficiency in water molecules under ambient conditions should not be considered for a single molecule only but rather for the whole cluster. At room temperature for a RH higher than 2%, there is a strong trend toward approximately occupying 2/3 of the three positions. For higher RH, the last third is progressively filled.
3.3. Classification of the Sesquihydrate
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
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Lemercier, A.; Couvrat, N.; Cartigny, Y.; Sanselme, M.; Corvis, Y.; Espeau, P.; Coquerel, G. Evidence of a New Crystalline Phase of Prednisolone Obtained from the Study of the Hydration–Dehydration Mechanisms of the Sesquihydrate. Pharmaceutics 2023, 15, 1694. https://doi.org/10.3390/pharmaceutics15061694
Lemercier A, Couvrat N, Cartigny Y, Sanselme M, Corvis Y, Espeau P, Coquerel G. Evidence of a New Crystalline Phase of Prednisolone Obtained from the Study of the Hydration–Dehydration Mechanisms of the Sesquihydrate. Pharmaceutics. 2023; 15(6):1694. https://doi.org/10.3390/pharmaceutics15061694
Chicago/Turabian StyleLemercier, Aurélien, Nicolas Couvrat, Yohann Cartigny, Morgane Sanselme, Yohann Corvis, Philippe Espeau, and Gérard Coquerel. 2023. "Evidence of a New Crystalline Phase of Prednisolone Obtained from the Study of the Hydration–Dehydration Mechanisms of the Sesquihydrate" Pharmaceutics 15, no. 6: 1694. https://doi.org/10.3390/pharmaceutics15061694
APA StyleLemercier, A., Couvrat, N., Cartigny, Y., Sanselme, M., Corvis, Y., Espeau, P., & Coquerel, G. (2023). Evidence of a New Crystalline Phase of Prednisolone Obtained from the Study of the Hydration–Dehydration Mechanisms of the Sesquihydrate. Pharmaceutics, 15(6), 1694. https://doi.org/10.3390/pharmaceutics15061694