Title |
A comprehensive spectroscopic study of the polymorphs of diflunisal and their phase transformations
|
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Published in |
International Journal of Pharmaceutics, June 2017
|
DOI | 10.1016/j.ijpharm.2017.06.020 |
Pubmed ID | |
Authors |
Anuradha R. Pallipurath, Francesco Civati, Juraj Sibik, Clare Crowley, J. Axel Zeitler, Patrick McArdle, Andrea Erxleben |
Abstract |
Understanding phase transitions in pharmaceutical materials is of vital importance for drug manufacturing, processing and storage. In this paper we have carried out comprehensive high-resolution spectroscopic studies on the polymorphs of the non-steroidal anti-inflammatory drug diflunisal that has four known polymorphs, forms I - IV (FI - FIV), three of which have known crystal structures. Phase transformations during milling, heating, melt-quenching and exposure to high relative humidity were investigated using Raman and terahertz spectroscopy in combination with differential scanning calorimetry and X-ray powder diffraction. The observed phase transformations indicate the stability order FIII > FI > FII, FIV. Furthermore, crystallization experiments from the gas phase and from solution by fast evaporation of different solvents were carried out. Fast evaporation of an ethanolic solution below 70°C was identified as a reliable and convenient method to obtain the somewhat elusive FII in bulk quantities. |
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Geographical breakdown
Country | Count | As % |
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Ireland | 2 | 33% |
United Kingdom | 2 | 33% |
Unknown | 2 | 33% |
Demographic breakdown
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Members of the public | 5 | 83% |
Scientists | 1 | 17% |
Mendeley readers
Geographical breakdown
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Unknown | 25 | 100% |
Demographic breakdown
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Student > Ph. D. Student | 7 | 28% |
Student > Bachelor | 3 | 12% |
Professor > Associate Professor | 3 | 12% |
Student > Doctoral Student | 2 | 8% |
Other | 2 | 8% |
Other | 4 | 16% |
Unknown | 4 | 16% |
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Pharmacology, Toxicology and Pharmaceutical Science | 5 | 20% |
Chemical Engineering | 2 | 8% |
Physics and Astronomy | 2 | 8% |
Medicine and Dentistry | 2 | 8% |
Other | 4 | 16% |
Unknown | 5 | 20% |