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Influence of Cooling Rate on Ice Crystallization and Melting in Sucrose-Water System
Malmö University, Sweden; Biofilms research center for Biointerfaces, Sweden; NextBioForm Competence Centre, Sweden.
RISE Research Institutes of Sweden, Bioeconomy and Health, Chemical Process and Pharmaceutical Development.ORCID iD: 0000-0001-9891-8968
Malmö University, Sweden; Biofilms research center for Biointerfaces, Sweden; NextBioForm Competence Centre, Sweden.
2022 (English)In: Journal of Pharmaceutical Sciences, ISSN 0022-3549, E-ISSN 1520-6017, Vol. 111, no 7, p. 2030-2037Article in journal (Refereed) Published
Abstract [en]

The ice crystallization and melting in systems where the equilibrium state is difficult to reach is one of the growing areas in pharmaceutical freeze-drying research. The quality of the final freeze-dried product depends on the parameters of the cooling step, which affect the ice nucleation and growth. In this paper, we present a DSC study of ice crystallization and melting in a sucrose-water system. Using two different types of thermal cycles, we examine the influence of cooling and heating rates on the thermal behavior of sucrose-water solutions with water contents between 50 and 100 wt%. The DSC results show that low cooling rates provide crystallization at higher temperatures and lead to lower amount of non-freezing water. Consequently, the glass transition and ice melting properties observed upon heating depend on the cooling conditions in the preceding step. Based on the experimental results, we investigate the reasons for the existence of the two steps on DSC heating curves in sucrose-water systems: the glass transition step and the onset of ice melting. We show that diffusion of water can be the limiting factor for ice growth and melting in the sucrose-water system when the amorphous phase is in a liquid state. In particular, when the diffusion coefficient drops below 10−14 m2/sec, the ice crystals growth or melting becomes strongly suppressed even above the glass transition temperature. Understanding the diffusion limitations in the sucrose-water system can be used for the optimization of the freeze-drying protocols for proteins and probiotics. © 2022 The Authors

Place, publisher, year, edition, pages
Elsevier B.V. , 2022. Vol. 111, no 7, p. 2030-2037
Keywords [en]
Crystallization, Differential scanning calorimetry (DSC), Diffusion, Excipients, Glass transition, Sucrose
National Category
Physical Chemistry
Identifiers
URN: urn:nbn:se:ri:diva-58785DOI: 10.1016/j.xphs.2022.01.027Scopus ID: 2-s2.0-85124515733OAI: oai:DiVA.org:ri-58785DiVA, id: diva2:1642081
Note

Funding text 1: This research was funded by the Swedish Governmental Agency for Innovation Systems (Vinnova) and was carried out within the competence center NextBioForm. We would like to express our gratitude for the valuable discussions and comments on the manuscript by Dr. Jonas Fransson (Nanexa AB, Sweden) who passed away in August 2021.

Available from: 2022-03-03 Created: 2022-03-03 Last updated: 2023-05-09Bibliographically approved

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Millqvist-Fureby, Anna

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