Morphology and growth control of griseofulvin recrystallized by compressed carbon dioxide as antisolvent

• Published in: Journal of crystal growth Vol. 262; no. 1; pp. 519 - 526
• Main Authors: De Gioannis, Barbara, Jestin, Patrick, Subra, Pascale
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 15.02.2004; Elsevier
• Subjects: A1. Crystal morphology; A2. GAS antisolvent recrystallization; A2. Growth from solutions; B1. Organic compounds; Cross-disciplinary physics: materials science; rheology; Exact sciences and technology; Growth from solutions; Materials science; Methods of crystal growth; physics of crystal growth; Physics; Theory and models of crystal growth; physics of crystal growth, crystal morphology and orientation; A2. GAS antisolvent recrystallization; A2. Growth from solutions; B1. Organic compounds; A1. Crystal morphology; Scanning electron microscopy; B1. Organic compound; Stirring; XRD; Griseofulvin; Experimental study; Particle size distribution; Morphology; Recrystallization; Crystal growth from solutions; Organic compounds
• ISSN: 0022-0248; 1873-5002
• DOI: 10.1016/j.jcrysgro.2003.10.025

Griseofulvin has been crystallized from acetone solutions using compressed carbon dioxide as antisolvent. Crystallization was performed in a batch stirred vessel at a temperature of 40°C and a final pressure of 100 bar. The effects of the antisolvent addition rate and of the stirring rate upon the morphology and size of the precipitated crystals were particularly investigated. Parameters were varied between 1.3–5.6 bar/min and 33–1000 rpm, respectively. Over the whole set of conditions, the product was obtained as tetragonal crystals with mean sizes from 40 μm to 20 mm. For a given CO 2 addition rate, the crystal morphology switched from a long needle to a bipyramid form as the stirring rate increased. For a given stirring rate and a given morphology, size of crystals decreased as the CO 2 addition rate increased. The rates also influenced the particle size distribution. The smallest size and narrowest particle size distribution were obtained at the highest stirring rate and antisolvent introduction rate, i.e. 1000 rpm and 5.6 bar/min, respectively.