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An experimental study on polymorph control and continuous heterogeneous crystallization of carbamazepine

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Abstract

Forms I–III and dihydrate carbamazepine (CBZ) were prepared and confirmed by X-ray powder diffraction (XRPD) and differential scanning calorimetry (DSC). Influences of supersaturation (σ), stirring, anti-solvent (H2O), and polymer type on the resultant polymorph are discussed. For a CBZ ethanol solution at 5 °C, more than 10 h was required to form crystals when σ was 0.5, while less than 2 s was required when σ was increased to 9.0. Very fine needle-shaped Form II crystals were obtained when σ ≥ 7.5. Higher stirring rates facilitated the formation of Form III CBZ. Continuous heterogeneous crystallization of Form III on polyvinyl alcohol (PVA, MW 89 000–98 000) was achieved in a one-stage mixed suspension mixed product removal (MSMPR) crystallizer at 15 °C and 300 rpm. At 5 °C and 40 rpm, only Form II crystals were obtained. However, Form II CBZ gradually transformed to Form III within 2 residence times, and the transition process was irreversible.

Graphical abstract: An experimental study on polymorph control and continuous heterogeneous crystallization of carbamazepine

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Publication details

The article was received on 12 Jun 2019, accepted on 11 Jul 2019 and first published on 11 Jul 2019


Article type: Paper
DOI: 10.1039/C9CE00908F
CrystEngComm, 2019, Advance Article

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    An experimental study on polymorph control and continuous heterogeneous crystallization of carbamazepine

    C. Hu, C. J. Testa, B. T. Shores, W. Wu, K. Shvedova, S. C. Born, S. Chattopadhyay, B. Takizawa and S. Mascia, CrystEngComm, 2019, Advance Article , DOI: 10.1039/C9CE00908F

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