Spray drying as a reliable route to produce metastable carbamazepine form IV

Rebecca A. Halliwell, Rajni M. Bhardwaj, Cameron Brown, Naomi E. B. Briggs, Jaclyn Dunn, John Robertson, Alison Nordon, Alastair J. Florence

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22 Citations (Scopus)
172 Downloads (Pure)


Carbamazepine is an active pharmaceutical ingredient used in the treatment of epilepsy that can form at least five polymorphic forms. Metastable form IV was originally discovered from crystallisation with polymer additives however has not been observed from subsequent solvent only crystallisation efforts. This work reports the reproducible formation of phase pure crystalline form IV by spray drying of methanolic carbamazepine solution. Characterisation of the material was carried out using diffraction, SEM and DSC. In situ Raman spectroscopy was used to monitor the spray dried product during the spray drying process. This work demonstrates spray drying provides a robust method for the production of form IV carbamazepine and the combination of high supersaturation and rapid solid isolation from solution overcomes the apparent limitation of more traditional solution crystallisation approaches to produce metastable crystalline forms.
Original languageEnglish
Pages (from-to)1874-1880
Number of pages7
JournalJournal of Pharmaceutical Sciences
Issue number7
Early online date19 Apr 2017
Publication statusE-pub ahead of print - 19 Apr 2017


  • spray drying
  • continuous processing
  • carbamazepine
  • metastable form
  • polymophism


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