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Preparation of microcrystals of piroxicam monohydrate by antisolvent precipitation via microfabricated metallic membranes with ordered pore arrays
journal contributionposted on 2017-11-22, 11:25 authored by Rahimah Othman, Goran VladisavljevicGoran Vladisavljevic, Elena Simone, Zoltan NagyZoltan Nagy, Richard Holdich
Microcrystals of piroxicam (PRX) monohydrate with a narrow size distribution were prepared from acetone/PRX solutions by antisolvent crystallisation via metallic membranes with ordered pore arrays. Crystallisation was achieved by controlled addition of the feed solution through the membrane pores into a well-stirred antisolvent. A complete transformation of an anhydrous form I into a monohydrate form of PRX was confirmed by Raman spectroscopy and differential scanning calorimetry. The size of the crystals was 7–34 μm and was controlled by the PRX concentration in the feed solution (15 −25 g L−1), antisolvent/solvent volume ratio (5–30), and the type of antisolvent (Milli-Q water or 0.1−0.5 wt% aqueous solutions of hydroxypropyl methyl2 cellulose (HPMC), polyvinyl alcohol or Pluronic P-123). The smallest crystals were obtained by injecting 25 g L−1 PRX solution through a stainless-steel membrane with a pore size of 10 μm into a 0.06 wt% HPMC solution stirred at 1,500 rpm using an antisolvent/solvent ratio of 20. HPMC provided better steric stabilisation of microcrystals against agglomeration than polyvinyl alcohol and Pluronic P-123, due to hydrogen bonding interactions with PRX and water. A continuous production of large PRX monohydrate microcrystals with a volume-weighted mean diameter above 75 μm was achieved in a continuous stirred membrane crystalliser. Rapid pouring of Milli-Q water into the feed solution resulted in a mixture of highly polydispersed prism-shaped and needle-shaped crystals.
The authors acknowledge the financial support for this work received from the Ministry of Higher Education in Malaysia, the Engineering and Physical Sciences Research Council (grant No. EP/HO29923/1) and the European Research Council (grant No. 280106-CrySys).
- Aeronautical, Automotive, Chemical and Materials Engineering
- Chemical Engineering
Published inCrystal Growth and Design
CitationOTHMAN, R. ...et al., 2017. Preparation of microcrystals of piroxicam monohydrate by antisolvent precipitation via microfabricated metallic membranes with ordered pore arrays. Crystal Growth and Design, 17, pp. 6692−6702.
PublisherAmerican Chemical Society (ACS)
- VoR (Version of Record)
Publisher statementThis work is made available according to the conditions of the Creative Commons Attribution 4.0 International (CC BY 4.0) licence. Full details of this licence are available at: http://creativecommons.org/licenses/by/4.0/
NotesThis is an open access article published under a Creative Commons Attribution (CC-BY) License, which permits unrestricted use, distribution and reproduction in any medium, provided the author and source are cited.