Preparation and characterization of Alendronate depot microspheres based on novel poly(-ε-caprolactone)/Vitamin E TPGS copolymers.

In the present study, new aledronate (AL) loaded microspheres were prepared with the use of polycaprolactone (PCL)/Vitamin E d-ɑ-tocopheryl poly(ethylene glycol) 1000 succinate (TPGS) copolymers. Specifically, PCL-TPGS copolymers, prepared at several PCL to TPGS ratios (namely, 90/10, 80/20, 70/30 and 60/40 w/w) via a ring opening polymerization process, were characterized by intrinsic viscosity, proton nuclear magnetic resonance (1H NMR), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), differential scanning calorimetry (DSC) and enzymatic hydrolysis. Results showed that as TPGS content increases the intrinsic viscosity of the copolymer (and hence, the viscosity-average molecular weight) is decreasing, while FTIR analysis showed the formation of hydrogen bonds between the -C[bond, double bond]O of PCL and the -OH of TPGS. Additionally, XRD analysis indicated that the prepared copolymers were semi-crystalline in nature, while enzymatic hydrolysis studies showed that increasing TGPS content led to increasing copolymer hydrolysis. In the following step, AL drug-loaded microspheres were prepared via single emulsification process. Scanning electron microscopy (SEM) revealed the formation of coarse drug-loaded microspheres with particle size close to 5 µm, while XRD analysis showed that the API was amorphously dispersed only in the cases of high TPGS content. Furthermore, FTIR analysis showed that the API did not interact with the copolymer components, while in vitro drug release studies showed that increasing PCL content led to decreasing API release rate. Finally, analysis of the drug release profiles suggested that the API release mechanism was solely governed by the polymer matrix erosion.

Novel Isocyanate-Modified Carrageenan Polymer Materials: Preparation, Characterization and Application Adsorbent Materials of Pharmaceuticals.

The present study focused on the synthesis and application of novel isocyanate-modified carrageenan polymers as sorbent materials for pre-concentration and removal of diclofenac (DCF) and carbamazepine (CBZ) in different aqueous matrices (surface waters and wastewaters). The polymer materials were characterized using Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Thermal Gravimetric Analysis (TGA) and Scanning Electron Microscopy (SEM). The effects on the adsorption behavior were studied, and the equilibrium data were fitted by the Langmuir and Freundlich models. The maximum adsorption capacity (Qmax) was determined by Langmuir⁻Freundlich model and was ranged for iota-carrageenan (iCAR) from 7.44 to 8.51 mg/g for CBZ and 23.41 to 35.78 mg/g for DCF and for kappa-carrageenan (kCAR) from 7.07 to 13.78 mg/g for CBZ and 22.66 to 49.29 mg/g for DCF. In the next step, dispersive solid phase extraction (D-SPE) methodology followed by liquid desorption and liquid chromatography mass spectrometry (LC/MS) has been developed and validated. The factors, which affect the performance of D-SPE, were investigated. Then, the optimization of extraction time, sorbent mass and eluent's volume was carried out using a central composite design (CCD) and response surface methodology (RSM). Under the optimized conditions, good linear relationships have been achieved with the correlation coefficient (R²) varying from 0.9901 to 0.995. The limits of detections (LODs) and limits of quantifications (LOQs) ranged 0.042⁻0.090 µg/L and 0.137⁻0.298 µg/L, respectively. The results of the recoveries were 70⁻108% for both analytes, while the precisions were 2.8⁻17.5% were obtained, which indicated that the method was suitable for the analysis of both compounds in aqueous matrices.