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Croker D.M.,Solid State Pharmaceutical Cluster | Croker D.M.,University of Limerick | Foreman M.E.,Solid State Pharmaceutical Cluster | Foreman M.E.,University College Cork | And 14 more authors.
Crystal Growth and Design | Year: 2012

A novel 1:1 cocrystal between p-toluenesulfonamide and triphenylphosphine oxide has been prepared and structurally characterized. This 1:1 cocrystal was observed to form during solid state grinding experiments, with subsequent formation of a known 3:2 cocrystal in the presence of excess sulfonamide. Both cocrystals are stable in the solid state. The ternary phase diagram for the two coformers was constructed in two different solvents: Acetonitrile and dichloromethane. Examination of these diagrams clarified solution crystallization of both the newly discovered 1:1 cocrystal and the previously reported 3:2 cocrystal, and identified regions of stability for each cocrystal in each solvent. The choice of solvent was found to have a significant effect on the position of the solid state regions within a cocrystal system. © 2011 American Chemical Society.

Croker D.M.,Solid State Pharmaceutical Cluster | Croker D.M.,University of Limerick | Hennigan M.C.,Solid State Pharmaceutical Cluster | Hennigan M.C.,National University of Ireland | And 8 more authors.
Journal of Pharmaceutical and Biomedical Analysis | Year: 2012

Diffraction and spectroscopic methods were evaluated for quantitative analysis of binary powder mixtures of FII(6.403) and FIII(6.525) piracetam. The two polymorphs of piracetam could be distinguished using powder X-ray diffraction (PXRD), Raman and near-infrared (NIR) spectroscopy. The results demonstrated that Raman and NIR spectroscopy are most suitable for quantitative analysis of this polymorphic mixture. When the spectra are treated with the combination of multiplicative scatter correction (MSC) and second derivative data pretreatments, the partial least squared (PLS) regression model gave a root mean square error of calibration (RMSEC) of 0.94 and 0.99%, respectively. FIII(6.525) demonstrated some preferred orientation in PXRD analysis, making PXRD the least preferred method of quantification. © 2012 Elsevier B.V..

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