4.7 Article

Spectroscopic characterization of single co-crystal of mefenamic acid and nicotinamide using supercritical CO2

Journal

JOURNAL OF MOLECULAR LIQUIDS
Volume 334, Issue -, Pages -

Publisher

ELSEVIER
DOI: 10.1016/j.molliq.2021.116117

Keywords

Co-crystallization; Single crystal; Supercritical carbon dioxide; X-ray diffraction; Infrared spectroscopy

Funding

  1. PHC Kolmogorov [N 41129RC]
  2. French Embassy in Kyiv in Ukraine
  3. Erasmus fellowship
  4. European Regional Development Fund (FEDER) [2S01059_IMODE]
  5. project ARCHICM, Chevreul Institute (FR 2638), Ministere de l'Enseignement Superieur et de la Recherche, Region Hauts-de-France

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This study successfully synthesized a single crystal of mefenamic acid and nicotinamide co-crystal using supercritical fluid, and determined the effect of temperature, solid mixture composition, and co-crystallization time on the synthesized solid, demonstrating the synthesis of the co-crystal.
The present study explores the possibility to synthetize, using supercritical fluid, single crystal of co-crystal formed by mefenamic acid as active pharmaceutical ingredient and nicotinamide as a co-former. The growth of single crystals is important for the determination of co-crystal structure and in particular, for the ones whose unit cells contain a large number of atoms, it becomes crucial. For this purpose, we analyzed the effect of temperature, solid mixture composition and time duration of the co-crystallization process on the synthetized solid. The structure of the latter was determined using single-crystal X-ray diffraction while the composition of fine powders and the intermolecular interactions involved in their synthesis were analyzed using powder X-ray diffraction and diffuse reflectance infrared Fourier transform spectroscopy respectively. Our results show that the single crystal of mefenamic acid and nicotinamide co-crystal is synthetized for the first time in supercritical CO2 at 90 degrees C, 193 bars and a time duration of three weeks. (C) 2021 Elsevier B.V. All rights reserved.

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