Effect of cocrystallization techniques on compressional properties of caffeine/oxalic acid 2:1 cocrystal

Abstract

Context: Caffeine/oxalic acid 2:1 cocrystal exhibited superior stability to humidity over caffeine, but compressional behavior is not studied yet. Objective: To compare compressional properties of caffeine/oxalic acid 2:1 cocrystal obtained by different cocrystallization techniques. Materials and methods: Cocrystal was obtained by solvent precipitation and ultrasound assisted solution cocrystallization (USSC) and characterized by X-ray powder diffraction and scanning electron microscopy. Compaction study was carried out at different compaction forces. Compact crushing strength, thickness and elastic recovery were determined. Results and discussion: Compaction was in order, caffeine > solvent precipitation cocrystal > USSC cocrystal. Caffeine exhibited sticking and lamination, where solvent precipitation compacts showed advantage. Caffeine and solvent precipitation compacts showed sudden drop in compactability, higher elastic recovery with severe lamination at 20,000 N. This was due to overcompaction. Crystal habit of two cocrystal products was same, but USSC cocrystals were difficult to compact. Uniform needle shaped USSC cocrystals must be difficult to orient in different direction and fracture during compression. Elastic recovery of USSC cocrystals was also more compared to other powders indicating less fracture and poor bonding between particles resulting in poor compaction. Conclusion: Cocrystal formation did not improve compressional property of caffeine. Cocrystals exposed to different crystallization environments in two techniques may have resulted in generation of different surface properties presenting different compressional properties.

Keywords::

• Caffeine
• compaction
• cocrystal
• ultrasound assisted solution cocrystallization
• elastic recovery
• mechanical property

Acknowledgments

Suyog Aher is thankful to Centre for Pharmaceutical Engineering Science, University of Bradford, Bradford, UK for providing research facilities.

Declaration of interest

We are very thankful to Centre for International Mobility (CIMO), Helsinki, Finland for providing the CIMO-India Fellowship (23.4.2010/TM-10-6968/Cimo India Fellowship). Suyog Aher is grateful to All India Council for Technical Education (AICTE, New Delhi, India) for providing financial support in the form of National Doctoral Fellowship (AICTE-NDF).