Spherical Crystallization of Glycine from Monodisperse Microfluidic Emulsions

Emulsion-based crystallization to produce spherical crystalline agglomerates (SAs) is an attractive route to control crystal size during downstream processing of active pharmaceutical ingredients (APIs). However, conventional methods of emulsification in stirred vessels pose several problems that li...

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Bibliographic Details
Published in:Crystal growth & design 2012-08, Vol.12 (8), p.3977-3982
Main Authors: Toldy, Arpad I, Badruddoza, Abu Zayed M, Zheng, Lu, Hatton, T. Alan, Gunawan, Rudiyanto, Rajagopalan, Raj, Khan, Saif A
Format: Article
Language:English
Subjects:
Condensed matter: structure, mechanical and thermal properties
Cross-disciplinary physics: materials science
rheology
Equations of state, phase equilibria, and phase transitions
Exact sciences and technology
Growth from melts
zone melting and refining
Materials science
Methods of crystal growth
physics of crystal growth
Physics
Solid-solid transitions
Specific phase transitions
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Summary:Emulsion-based crystallization to produce spherical crystalline agglomerates (SAs) is an attractive route to control crystal size during downstream processing of active pharmaceutical ingredients (APIs). However, conventional methods of emulsification in stirred vessels pose several problems that limit the utility of emulsion-based crystallization. In this paper, we use capillary microfluidics to generate monodisperse water-in-oil emulsions. Capillary microfluidics, in conjunction with evaporative crystallization on a flat heated surface, enables controllable production of uniformly sized SAs of glycine in the 35–150 μm size range. We report detailed characterization of particle size, size distribution, structure, and polymorphic form. Further, online high-speed stereomicroscopic observations reveal several clearly demarcated stages in the dynamics of glycine crystallization from emulsion droplets. Rapid droplet shrinkage is followed by crystal nucleation within individual droplets. Once a nucleus is formed within a droplet, crystal growth is very rapid (
ISSN:1528-7483
1528-7505
DOI:10.1021/cg300413s