Polymorphism in the co-crystallization of the anticonvulsant drug carbamazepine and saccharin using supercritical CO2 as an anti-solvent
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2018
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Elsevier
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Cuadra IA, Cabañas A, Cheda JAR, Pando C. Polymorphism in the co-crystallization of the anticonvulsant drug carbamazepine and saccharin using supercritical CO 2 as an anti-solvent . Journal of Supercritical Fluids. 2018;136:60-9.
Abstract
1:1 Co-crystals of carbamazepine (CBZ) and saccharin (SAC) were obtained for the first time through the supercritical anti-solvent (SAS) technique based on using supercritical CO2 as anti-solvent. The capability of SAS to produce the desired polymorphic form (two polymorphs are known) was assessed. Operational conditions investigated were temperature (40.0 and 60.0 °C), pressure (10.0 and 15.0 MPa), solvent choice and coformer concentration in the organic solution (CBZ: 30 and 15 mg/mL; SAC: stoichiometric ratio). Co-crystals were characterized in terms of crystallinity and coformers interactions. No homocrystals were present. Using methanol, at 40.0 °C polymorph I was obtained with yields up to 65%; whilst at 60.0 °C a mixture of polymorphs was obtained. Mixtures of polymorphs were also obtained in the ethanol and dichloromethane experiments at the studied conditions while the dimethylsulfoxide experiments failed to produce any co-crystal polymorph. For comparison purposes, pure CBZ and SAC were also processed by SAS.