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The Physical Stability of Felodipine and Its Recrystallization from an Amorphous Solid Dispersion Studied by NMR Relaxometry

  • Research Article
  • Theme: Advancements in Amorphous Solid Dispersions to Improve Bioavailability
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Abstract

The 1H nuclear magnetic resonance (NMR) relaxometry method was applied to investigate the physical stability of an active pharmaceutical ingredient (API) and, for the first time, its recrystallization process in an amorphous solid dispersion system (ASD). The ASD of felodipine and polyvinylpyrrolidone (PVP) was prepared using the solvent evaporation method in a mass ratio of 50:50. In the first stage of the study (250 days), the sample was stored at 0% relative humidity (RH). The recovery of magnetization was described by one-exponential function. In the second stage (300 days in 75% relative humidity), the recrystallization process of felodipine was studied, showing in the sample three components of equilibrium magnetization related to (i) crystalline felodipine, (ii) water, and (iii) felodipine and PVP remaining in the ASD. The study shows that the 1H NMR relaxometry method is a very useful tool for analysing the composition of a three-phase system mixed at the molecular level and for the investigation of recrystallization process of API in amorphous solid dispersion system.

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Funding

The work was part-financed by the Plenipotentiary of Poland to JINR, Dubna, Program “A study of the structure and molecular dynamics in crystalline and amorphous therapeutic compounds.”

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Authors and Affiliations

  1. Department of Medical Physics and Radiospectroscopy, Faculty of Physics, Adam Mickiewicz University, Uniwersytetu Poznańskiego 2, 61-614, Poznan, Poland

    A. Pajzderska & J. Wąsicki

  2. Department of Inorganics and Analytical Chemistry, Poznań University of Medical Sciences, Grunwaldzka 6, 60-780, Poznan, Poland

    J. Mielcarek

  3. NanoBioMedical Centre, Adam Mickiewicz University, Wszechnicy Piastowskiej 3, 61-614, Poznan, Poland

    J. Wąsicki

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  1. A. Pajzderska
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Contributions

AP and JW contribute to the conceptualization and design of the work. The samples were prepared by JM. AP performed all of the experiments and data acquisition. Data was analyzed and visualized by AP and JW. The original draft was written by JW, while AP and JM helped with review and editing. All authors have read and agreed to the published version of the manuscript.

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Correspondence to A. Pajzderska.

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Pajzderska, A., Mielcarek, J. & Wąsicki, J. The Physical Stability of Felodipine and Its Recrystallization from an Amorphous Solid Dispersion Studied by NMR Relaxometry. AAPS PharmSciTech 23, 93 (2022). https://doi.org/10.1208/s12249-022-02234-8

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