Degradation of azithromycin using Ti/RuO<Subscript>2</Subscript> anode as catalyst followed by DPV,HPLC–UV and MS analysis

The electrodegradation of azithromycin was studied by its indirect oxidation using dimensionally stable Ti/RuO₂ anode as catalyst in the electrolyte containing methanol, 0.05 M NaHCO₃, sodium chloride and deionized water. The optimal conditions for galvanostatic electrodegradation for the azithromycin concentration of 0.472 mg cm^?3 were found to be NaCl concentration of 7 mg cm^?3 and the applied current of 300 mA. The differential pulse voltammetry using glassy carbon electrode was performed for the first time in the above-mentioned content of electrolyte for the nine concentration of azithromycin (0.075–0.675 mg cm^?3) giving the limits of azithromycin detection and of quantification as: LOD 0.044 mg cm^?3 and LOQ 0.145 mg cm^?3. The calibration curve was constructed enabling the electrolyte analysis during its electrodegradation process. The electrolyte was analyzed by high-performance liquid chromatography and electrospray ionization time-of-flight mass spectrometry. The electrooxidation products were identified and after 180 min there was no azithromycin in the electrolyte while TOC analysis showed that 79% of azithromycin was mineralized. The proposed degradation scheme is presented.     

Discontinuous alkylation of diphenylamine with nonene for maximum catalyst utilization

This study examines the alkylation of diphenylamine (DPA) with nonene (NON) in a liquid phase catalyzed by acid-treated clay-based catalysts from commercial suppliers (Fulcat 22B, Nobelin MM, and Jeltar 300). Alkylations were conducted to achieve the highest possible selectivity of diisononyldiphenylamine (DNDPA), low selectivity of monoisononyldiphenylamine, and a maximum triisononyldiphenylamine yield of 4%. This study also examines the reaction conditions to selectively form dialkylated diphenylamine from DPA and NON in a batch reactor. Repeated use of the catalyst during the alkylation of DPA with NON was also investigated. Catalyst deactivation takes place during the alkylation of each batch and intensifies with repeated catalyst use, resulting in low DNDPA selectivity. The regenerated catalyst was sufficiently active only until the regeneration of the first and second batches. After the third batch, the catalyst’s selectivity for DNDPA was very low, and its reuse in the alkylation of DPA with NON was not efficient. Therefore, to achieve the maximum length of catalyst activity, the fresh catalyst was gradually added to the used catalyst from a previous batch, thus maintaining a high activity of eight batches. The reduction in catalyst activity was probably caused by the irreversible adsorption of substances on the surface, a loss of microporous structure, and a loss of surface acidity. DPA or alkylated products are adsorbed on the surface oxygen of the catalyst through nitrogen and form nitro formations. The fresh and regenerated catalysts were characterized by their surface area, surface acidity, pore size distribution, and pore volume.     

Utilization of GDOES for the study of friction layers formed on the surface of brake discs during the friction process

The paper deals with the chemical characterization of friction layer, generated on the surface of friction materials during the friction test using the glow discharge optical emission spectrometry (GDOES). Friction layer is formed during the friction process and its character depends on several factors. One of the most important factors is the material composition of brake pads and brake disc. When the brake pressure is released at the end of the braking event, the specific friction layer remains on the surface of both pairs (brake pads and brake disc). Using the GDOES profile analysis, the thicknesses of friction layers were estimated and these results were compared with results obtained by scanning electron microscopy together with X-ray microanalysis.     

Performance improvement of PDMS/PES membrane by adding silicalite-1 nanoparticles: separation of xenon and krypton

The polydimethylsiloxane (PDMS) mixed matrix membrane with dispersed phase of nanozeolite silicalite-1 has been synthesized on polyethersulphone (PES) as a support, and its performance in the gas separation of xenon and krypton has been studied. For this purpose, nanozeolite silicalite-1 is synthesized by the hydrothermal clear solution method and is characterized by XRD and SEM analysis. In this research, the separation performance of MMM has also been compared with the polymeric PDMS membrane. Furthermore, the effect of feed pressure and loading percentage of nanozeolite in the polymeric matrix are evaluated. The results indicate that the addition of nanozeolite to the polymeric matrix improves its separation performance, and that the changes of the feed pressure have no major effect. The average permeability of the krypton and xenon gases through the PDMS polymeric membrane is calculated as 1.25 × 10^?9 and 1.78 × 10^?9 cm mol/(cm² s kPa), respectively, while by adding only 5 wt% of nanosilicalite-1 to the polymeric matrix of the membrane, this amount increased to 1.82 × 10^?9 and 8.07 × 10^?9 cm mol/(cm² s kPa), respectively. In addition, the presence of nanosilicalite-1 as the filler leads to an increase in the selectivity of xenon to krypton up to 4.38.     

Microemulsion high performance liquid chromatography method for the determination of ibuprofen in the presence of preservatives and impurities in oral pediatric suspension

A simple and rapid isocratic oil-in-water microemulsion HPLC method (MELC) has been developed for the analysis of ibuprofen in oral suspension formulation. The method was optimized for simultaneous separation and determination of Ibuprofen and its related compound C (Imp C), sodium benzoate, methylparaben, propylparaben and their related compound A (Imp A). The optimum conditions were achieved by testing several columns and mobile phase compositions, while the chromatographic parameters (retention time, plate number, tailing factor and resolution) were measured. The six compounds were successfully separated within a run time of 14 min, using Eurospher II C18 (150 mm × 4.6 mm i.d., 5 µm) at ambient temperature, a mobile phase made of 5.0 g SDS, 6.6 g butan-1-ol, 0.8 g n-heptane in 100 mL of 0.05% TFA. Flow rate was fixed to 1 mL min^?1 and wavelength detection to 254 nm. The same phase was used in UHPLC and monolithic columns. A rapid comparison of system suitability between the three methods was made. The HPLC method was validated following ICH guidelines in terms of selectivity, linearity, accuracy and precision. The developed method was successfully applied to a commercial pharmaceutical formulation which shows that it can be used for routine analysis.     

Synthesis and in vitro antibacterial evaluation of 6-substituted 4-amino-pyrazolo[3,4-<Emphasis Type="Italic">d</Emphasis>]pyrimidines

Pyrazolo[3,4-d]pyrimidines are one of the most important classes of fused heterocyclic compounds which exhibit a broad range of biological and medicinal properties. They are known as anticancer, antifungal, antibacterial, antiviral and anti-inflammatory agents. In this study, some new 6-substituted 4-amino-pyrazolo[3,4-d]pyrimidine derivatives were prepared via reaction of 5-amino-3-methyl-1-phenyl-1H-pyrazole-4-carbonitrile with various nitriles in the presence of sodium ethoxide as catalyst. The inhibitory properties of synthesized compounds were studied according to CLSI guidelines against some pathogenic bacteria including four gram-positive strains (Streptococcus pyogenes, Staphylococcus aureus, Bacillus cereus and Bacillus subtilis subsp. spizizenii) and three gram-negative strains (Pseudomonas aeruginosa, Shigella flexneri and Salmonella enterica subsp. enterica). The antibacterial effects of all derivatives were compared with those of antibiotics belonging to different classes. The values were reported as inhibition zone diameter (IZD), minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC). The effect of substituents on the biological activity of derivatives was discussed as well. The inhibitory effect of compound 6a, was shown to be the most, with MIC values in the range of 32–4096 μg/mL. Since most of the synthesized compounds were effective against Streptococcus pyogenes and Pseudomonas aeruginosa, they can be considered as inhibitors of these two bacteria.     

Oxidative degradation of levofloxacin by water-soluble manganese dioxide in aqueous acidic medium: a kinetic study

Pharmaceuticals, especially fluoroquinolone antibiotics, have received increasing global concern, due to their intensive use in the environment and potential harm to ecological system as well as human health. Degradation of antibiotics, such as oxidative degradation by metal oxides, often plays an important role in the elimination of antibiotics from the environment. The kinetics of oxidation of levofloxacin by water-soluble manganese dioxide has been studied in aqueous acidic medium at 25 °C temperature. The stoichiometry for the reaction indicates that the oxidation of 1 mol of levofloxacin requires 1 mol of manganese dioxide. The reaction is second order, that is first order with respect to manganese dioxide and levofloxacin. The rate of reaction increases with the increasing [H⁺] ion concentration. A probable reaction mechanism, in agreement with the observed kinetic results, has been proposed and discussed. The energy and enthalpy of activation have been calculated to be 30.54 and 28.07 kJ mol^?1, respectively.     

The optical properties of a novel metal-free phthalocyanine

In the present work, 4-(4′-dodecyloxycarbonyl) phenoxy phthalonitrile was synthesized and then this phthalonitrile derivative was cyclotetramerized in dodecanol resulting a new metal-free phthalocyanine. The optical properties of this phthalocyanine were investigated. Novel metal-free phthalocyanine thin films were deposited on indium tin oxide-coated glass substrates by spinning method. Surface and microstructural properties of the films were characterized by atomic force microscopy and scanning electron microscopy. Both the transmittance and reflectance spectra of the deposited films were recorded using an NKD analyser. The optical band gap energy, the thickness of thin films, refractive index (n) and extinction coefficient (k) were calculated as 2.7 eV, 300 nm, 1.47 and 0.02, respectively.