Probing fluconazole deposition inside mesoporous silica using solid-state NMR spectroscopy: Crystallization of a confined metastable form and phase transformations under storage conditions.

Encapsulation of molecules into mesoporous silica carriers continues to attract considerable interest in the area of drug delivery and crystal engineering. Here, MCM-41, SBA-15 and MCF silica matrices were used to encapsulate fluconazole (FLU), a pharmaceutically relevant molecule with known conformational flexibility, using the melting method. The composites have been characterized using 1H, 13C and 19F NMR spectroscopy, nitrogen adsorption, PXRD and thermal analysis (DSC, TGA). Drug loading up to 50 wt% allowed us to probe the crystallization process and to detect different local environments of confined FLU molecules. 19F NMR spectroscopy enabled us to detect the gradual pore filling of silica with FLU and differentiate the amorphous domains and surface species. The use of the complementary structural and thermal techniques enabled us to monitor crystallization of the metastable FLU form II in MCF. Using 1H and 19F NMR spectroscopy we observed pore-size dependent reversible dehydration/hydration behaviour in the MCM and SBA composites. As water content has considerable importance in understanding of physicochemical stability and shelf-life of pharmaceutical formulations, experimental evidence of the effect of API-water-carrier interactions on the API adsorption mechanism on silica surface is highlighted.

The effect of spent bleaching earth ageing process on its physicochemical and microbial composition and its potential use as a source of fatty acids and triterpenes.

This study was aimed at investigating the physicochemical and microbiological changes that took place during the ageing process of spent bleaching earth in the presence of autochthonous microorganisms. Research material included fresh spent bleaching earth (SBE0) and the same material after 3 years of storage at the constant temperature of 20 °C, without aeration and moistening (SBE3). Changes in the chemical composition of analysed waste material were observed during its ageing process point to a spontaneous bioconversion of fat substance towards formation and/or release of free saturated fatty acids C16:0 and C18:0 (14.3 g 100 g(-1) D.M.), triterpenes (8.48 g 100 g(-1) D.M.), cholesterol (3.29 g 100 g(-1) D.M.), small quantities of carbohydrates and esters (0.80 g 100 g(-1) D.M.). This process was accompanied by other changes in physicochemical parameters of the waste material, such as colour, odour and viscosity, decrease in fat content from 28.27 to 24.6 % and that of soluble forms of metals (Mo, Cu, Fe, Zn, Ni, Cr and Mn), ranging from 25 to 75 %, and an increase in pH, from 3.85 to 4.2. At the same time, changes in the microbial consortium were observed.