MS05-P10 Towards understanding phase transitions of confined pharmaceuticals Alexander Morritt (School of Pharmacy, University of East Anglia, Norwich, United Kingdom) Karol Nartowski (Wroclaw Medical University, Wrocław, Poland) László Fábián (School of Pharmacy, University of East Anglia, Norwich, United Kingdom) Yaroslav Khimyak (School of Pharmacy, University of East Anglia, Norwich, United Kingdom)email: change in the phases of matter has been extensively studied; from simplistic thermal changes of liquids, solids and gases to more the complex transitions of the different forms of the same material. This is important for pharmaceuticals because different polymorphs of the same drug having different intrinsic properties such as solubility and bioavailability. In studying these systems it is difficult to isolate different phases of matter in the early stages of crystallisation, as when these transitional phases occur they have a limited lifetime. Therefore stopping/slowing microscale crystallisation in order to observe the early stages is the aim of this project. This is achieved by encapsulating the pharmaceutical into a host with confined nanoscale geometry, in this case a mesoporous silica host. This allows for an indirect route into understanding relationships between different phases and motilities of pharmaceutical materials. Melt loading methods were used to in order to encapsulate the cocrystal of flufenamic acid and nicotinamide (FFA/NA) within the pores. Confirmation of loading at different ratios inside the pore was completed using DSC, nitrogen desorption isotherms. Subsequent NMR analysis was completed by solid state NMR methods to investigate the 1H, 13C and 19F environments by different correlation experiments under MAS conditions. Defined separate phase peaks using 19F NMR were observed previously in this material; surface, crystalline and amorphous peaks. Using 19F-19F NOESY NMR, interactions between these peaks were observed giving two out of the possible three interactions giving insight into spatial differences between the different phases of material.References:

Nartowski, K. P. et al. (2015). Phys. Chem. Phys. 17, 24761-24773

Nartowski, K. P. et al. (2016) Angew. Chemie. Int. Ed. 55, 8904-8908
Keywords: phase, NMR, pharmaceuticals