Effects of TiO2 Nanoparticles Synthesized via Microwave Assistance on Adsorption and Photocatalytic Degradation of Ciprofloxacin.

In this study, the optimal microwave-assisted sol-gel synthesis parameters for achieving TiO2 nanoparticles with the highest specific surface area and photocatalytic activity were determined. Titanium isopropoxide was used as a precursor to prepare the sol (colloidal solution) of TiO2. Isopropanol was used as a solvent; acetylacetone was used as a complexation moderator; and nitric acid was used as a catalyst. Four samples of titanium dioxide were synthesized from the prepared colloidal solution in a microwave reactor at a temperature of 150 °C for 30 min and at a temperature of 200 °C for 10, 20, and 30 min. The phase composition of the TiO2 samples was determined by X-ray diffraction analysis (XRD) and Fourier-transform infrared spectroscopy (FTIR). Nitrogen adsorption/desorption isotherms were used to determine the specific surface area and pore size distributions using the Brunauer-Emmett-Teller (BET) method. The band-gap energy values of the TiO2 samples were determined by diffuse reflectance spectroscopy (DRS). The distribution of Ti and O in the TiO2 samples was determined by SEM-EDS analysis. The effects of adsorption and photocatalytic activity of the prepared TiO2 samples were evaluated by the degradation of ciprofloxacin (CIP) as an emerging organic pollutant (EOP) under UV-A light (365 nm). The results of the photocatalytic activity of the synthesized TiO2 nanoparticles were compared to the benchmark Degussa P25 TiO2. Kinetic parameters of adsorption and photocatalysis were determined and analyzed. It was found that crystalline TiO2 nanoparticles with the highest specific surface area, the lowest energy band gap, and the highest photocatalytic degradation were the samples synthesized at 200 °C for 10 min. The results indicate that CIP degradation by all TiO2 samples prepared at 200 °C show a synergistic effect of adsorption and photocatalytic degradation in the removal process.

Optimization of Ciprofloxacin Adsorption on Clinoptilolite-Based Adsorbents Using Response Surface Methodology.

The adsorption of the antibiotic ciprofloxacin (CIP) from water solution by natural zeolite-clinoptilolite (CLI), magnetic clinoptilolite (MAG-CLI), and graphene oxide coated magnetic clinoptilolite (GO-MAG-CLI) was investigated. The novel approach of an environmentally friendly and cost-effective microwave-assisted method was applied for the magnetic composite synthesis. Detailed characterization of the prepared composites was achieved. In order to investigate the effect of the initial CIP concentration, pH, temperature, contact time, and type of adsorbent on the adsorption efficiency of CIP, and to obtain the optimal conditions for CIP removal, the response surface methodology central composite factorial design (RSM-CCF) was applied. The results obtained by the RSM-CCF showed that among the studied adsorbents, GO-MAG-CLI had the highest adsorption capacity for CIP, achieved for the initial concentration of 48.47 mg dm-3 at a pH of 5 and 24.78 °C after 19.20 min of contact time. The adsorption kinetics studied for the initial CIP concentration range of 15-50 mg dm-3 followed Lagergren's pseudo-second-order model, and the Langmuir isotherm was the most suitable one to describe the CIP adsorption onto GO-MAG-CLI.

Rapid Microwave-Assisted Synthesis of N/TiO2/rGO Nanoparticles for the Photocatalytic Degradation of Pharmaceuticals.

Nanocomposites comprising nitrogen-doped TiO2 and reduced graphene oxide (N/TiO2/rGO), with different rGO loading qualities, were prepared by a cost-effective microwave-assisted synthesis method. The synthesized materials were broadly characterized by Raman spectroscopy, X-ray diffraction (XRD), infrared spectroscopy (FTIR), photoelectron spectroscopy (XPS), diffuse reflectance spectroscopy (DRS), electron microscopy (SEM-EDS), and nitrogen adsorption/desorption isotherms. Anatase was the only crystalline phase observed for all synthesized materials. The rGO loading did not affect the morphological properties, but it positively influenced the photocatalytic activity of the nanocomposite materials, especially at low rGO loading. Photocatalysts were evaluated via the degradation of specific organic micropollutant (OMP) pharmaceuticals: ciprofloxacin (CIP), diclofenac (DCF), and salicylic acid (SA), under different radiation sources: ultraviolet A (UVA), solar light simulator (SLS), blue visible light (BVL) and cold visible light (CVL). CIP and SA were removed effectively via the synergy of adsorption and photocatalysis, while DCF degradation was achieved solely by photocatalysis. After implementing scavenger agents, photocatalytic degradation processes mainly depended on the specific pollutant type, while irradiation sources barely defined the photocatalytic mechanism. On the other hand, changes in irradiation intensity significantly influenced the photolysis process, while photocatalysis was slightly affected, indicating that irradiation spectra are more relevant than intensity.

Tailoring functional spray-dried powder platform for efficient donepezil nose-to-brain delivery.

Shortcomings of oral donepezil administration in the treatment of Alzheimer's disease have paved the way for ongoing investigations towards more efficient and safe donepezil nose-to-brain delivery. Herein we present the development of advantageous powder platform for donepezil nose-to-brain delivery, coupling careful design of chitosan and mannitol-based carrier matrix with spray-drying technology advantages and early consideration of adequate nasal administration mode, employing QbD approach. Unprecedentedly, ultrasonic nozzle was used to atomise the drying feed in response to size-related requirements for nasal aerosol particles. The optimised spray-drying process resulted in free-flowable dry powder with a great majority of particles larger than 10 µm, ensuring localised nasal deposition upon aerosolization, as evidenced by using 3D-printed nasal cavity model. QbD approach coupling formulation, process and administration parameters enabled optimisation of drug deposition profile reaching tremendously high 65.5 % of the applied dose deposited in the olfactory region. The leading formulation exhibited favourable swelling, mucoadhesion, drug release and permeation-enhancing properties, suiting the needs for efficient brain-targeted delivery. Results of in vitro biocompatibility and physico-chemical stability studies confirmed the leading formulation potential for safe and efficient donepezil nose-to-brain delivery. The obtained results encourage extending the study to an appropriate in vivo model needed for the final proof-of-concept.

Microwave-Assisted Synthesis of N/TiO2 Nanoparticles for Photocatalysis under Different Irradiation Spectra.

Nitrogen-doped TiO2 (N/TiO2) photocatalyst nanoparticles were derived by the environmentally friendly and cost-effective microwave-assisted synthesis method. The samples were prepared at different reaction parameters (temperature and time) and precursor ratio (amount of nitrogen source; urea). The obtained materials were characterized by X-ray diffraction (XRD), photoelectron spectroscopy (XPS), Raman spectroscopy (RS), infrared spectroscopy (FTIR), diffuse reflectance spectroscopy (DRS), electron microscopy (SEM-EDS), and nitrogen adsorption/desorption isotherms. Two cycles of optimizations were conducted to determine the best reaction temperature and time, as well as N content. The phase composition for all N/TiO2 nanomaterials was identified as photoactive anatase. The reaction temperature was found to be the most relevant parameter for the course of the structural evolution of the samples. The nitrogen content was the least relevant for the development of the particle morphology, but it was important for photocatalytic performance. The photocatalytic activity of N/TiO2 nanoparticle aqueous suspensions was evaluated by the degradation of antibiotic ciprofloxacin (CIP) under different irradiation spectra: ultraviolet A light (UVA), simulated solar light, and visible light. As expected, all prepared samples demonstrated efficient CIP degradation. For all irradiation sources, increasing synthesis temperature and increasing nitrogen content further improved the degradation efficiencies.

Preparation of Filaments and the 3D Printing of Dronedarone HCl Tablets for Treating Cardiac Arrhythmias.

The production of 3D-printed dosage forms requires the preparation of high-quality filaments containing an active pharmaceutical ingredient (API). The objective of this research is to prepare filaments containing dronedarone hydrochloride, a drug used in the treatment of cardiac arrhythmias. Filaments and 3D-printed tablets were subjected to characterization methods in order to prove and ensure the stability of the API and preservation of the drug content. Blends containing different proportions of dronedarone hydrochloride (DNR), polyethylene glycol (PEG), and polyvinyl alcohol filament (PVA) were prepared in two forms: as a powder mixture and as a solid dispersion. Thermogravimetric analysis was conducted, and the thermal properties of the components and polymer blends were tested using differential scanning calorimetry. Hot melt extrusion at 170 °C was used to prepare the filaments, and the fused deposition modeling technique was employed to print tablets. Drug release profiles were obtained by in vitro tests. The results indicate that the mixture containing 10 wt.% of polyethylene glycol prepared as a solid dispersion exhibits the most straightforward structure and shows only the slightest deviation from the target filament diameter. The compact structure of the tablet obtained from the filament provides a uniform in vitro drug release over a 24-h period. It also shows the smallest aberration from the expected DNR content in the tablet. The paper demonstrates that a blend containing 10 wt.% of PEG, 10 wt.% of DNR, and 80 wt.% of PVA filament is the most appropriate formula for extrusion and tablet printing.