Microcrystals of piroxicam (PRX) monohydrate with a narrow size distribution were prepared from acetone/ PRX solutions by antisolvent crystallization via metallic membranes with ordered pore arrays. Crystallization 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 type of antisolvent (Milli-Q water or 0.1−0.5 wt % aqueous solutions of hydroxypropyl methyl cellulose (HPMC), poly(vinyl 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 1500 rpm using an antisolvent/solvent ratio of 20. HPMC provided better steric stabilization of microcrystals against agglomeration than poly(vinyl 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 crystallizer. Rapid pouring of Milli-Q water into the feed solution resulted in a mixture of highly polydispersed prism-shaped and needle-shaped crystals.
Preparation of microcrystals of piroxicam monohydrate by antisolvent precipitation via microfabricated metallic membranes with ordered pore arrays / Othman, R.; Vladisavljevic, G. T.; Simone, E.; Nagy, Z. K.; Holdich, R. G.. - In: CRYSTAL GROWTH & DESIGN. - ISSN 1528-7483. - 17:12(2017), pp. 6692-6702. [10.1021/acs.cgd.7b01307]
|Titolo:||Preparation of microcrystals of piroxicam monohydrate by antisolvent precipitation via microfabricated metallic membranes with ordered pore arrays|
|Data di pubblicazione:||2017|
|Digital Object Identifier (DOI):||http://dx.doi.org/10.1021/acs.cgd.7b01307|
|Appare nelle tipologie:||1.1 Articolo in rivista|
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