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Issue 34, 2019
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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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Supplementary files

Article information


Submitted
12 Jun 2019
Accepted
11 Jul 2019
First published
11 Jul 2019

CrystEngComm, 2019,21, 5076-5083
Article type
Paper
Author version available

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, 21, 5076
DOI: 10.1039/C9CE00908F

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