Sunitinib malate, as an anticancer compound and a multi-targeted tyrosine-kinase inhibitor for treatment of glioma, was comprehensively studied by using different liquid chromatography methods. Since sunitinib malate shows Z-E isomerism, various reverse phase high performance liquid chromatography (RP-HPLC) programs were designed to access quantitative determination and good separation of Z-E stereoisomers. Moreover, some impurities including N-oxide and impurity B were to be separated from the main isomer with acceptable resolution. In the present work, different RP-HPLC programs were developed in which the type of mobile phase, flow rate, pH, and temperature were optimized to reach the best analysis conditions and control the rate of Z to E conversion. In addition, the effect of some operational parameters during the solution preparation including initial concentration of the analyte, temperature, pH, and type of solvent on the stability of Z isomer were investigated. The opted conditions for quantitative analysis were C8-Hector column as stationary phase, methanol as solvent, ammonium acetate buffer containing triethylamine as mobile phase, the pH of mobile phase of 8.5, the flow rate of 1.0 mL/min, and detection at 425 nm. In this situation the peaks of E and Z isomers were at 16.3 and 19.7 min. Full validation of the designed method was done based on ICH guidelines. 相似文献
Fe3O4 magnetic nanoparticles (MNPs) were prepared by co-precipitation method. The nanoparticles were silica coated using TEOS, and then modified by the polymeric layers of polypropylene glycol (PPG) and polyethylene glycol (PEG). Finally, the core-shell samples were decorated with Ag, Au, and Cu nanoparticles. The products were characterized by vibrating sample magnetometry (VSM), TGA, SEM, XRD, and FTIR methods. The antibacterial activity of the prepared samples was evaluated in inactivation of E. coli and S. aureus microorganisms, representing the Gram-negative and Gram-positive species, respectively. The effect of solid dosage, bacteria concentration and type of polymeric modifier on the antibacterial activity was investigated. TEM images of the bacteria were recorded after the treatment time and according to the observed changes in the cell wall, the mechanism of antibacterial action was discussed. The prepared nanostructures showed high antibacterial activity against both Gram-negative and Gram-positive bacteria. This was due to the leaching of metal ions which subsequently led to the lysis of bacteria. A theoretical investigation was also done by studying the interaction of loaded metals with the nucleotide components of the microorganism DNA, and the obtained results were used to explain the experimental data. Finally, based on the observed inactivation curves, we explain the antibacterial behavior of the prepared nanostructures mathematically.
Zeolite-based photocatalysts were prepared by the sol-gel and deposition methods. The photocatalysts were characterised by
X-ray diffraction, nitrogen adsorption-desorption isotherms, FTIR spectroscopy, scanning electron microscopy and energy-dispersive
X-ray spectrometry. The activity of the prepared photocatalysts was evaluated by the UV-induced degradation of acid blue 92,
a textile dye in common use. The effect of various parameters, such as catalyst concentration, initial dye concentration,
thiosulphate concentration and pH, on the rate and efficiency of the photocatalytic degradation of acid blue 92 was investigated.
The results showed that each parameter influenced the degradation rate and efficiency in a particular way. It was also found
that, under optimised conditions, Ag/AgBr/TiO2/zeolite exhibited the highest photocatalytic performance. A comparison of catalytic activity when exposed to visible light
under the same conditions showed that the photocatalysts containing AgBr had the highest activity. 相似文献
XFe2O4 magnetic nanoparticles (X = Mn, Fe, Co, Ni, and Zn) were prepared by using two methods: coprecipitation and hydrothermal. The synthesized nanoparticles were compared according to the separation in an external magnetic field and finally, the hydrothermal method was specified as a better synthesis method. The magnetic nanoparticles were characterized by physico-chemical analysis methods such as Vibrating Sample Magnetometer (VSM), X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy (FTIR), nitrogen adsorption-adsorption isotherm and Transmission Electron Microscopy (TEM). Magnetic properties of synthesized nanoparticles were studied by ab-initio theoretical methods to confirm and compare with the experimental results. According to the VSM analysis, all of magnetic nanoparticles had good magnetization while CoFe2O4 nanoparticles showed the ferromagnetic behavior. The magnetic properties of XFe2O4 configurations were studied using Density Functional Theory ab-initio method. The theoretical results were consistent with experimental magnetizations in the absence of external field. Finally, the photocatalytic behavior of prepared samples was investigated in the presence of oxone as an accelerated agent for degradation of an azo dye. 相似文献
Mordenite (MOR) nanocrystals were synthesized using the hydrothermal method. Sol–gel and deposition methods were utilized to modify the zeolite surface with TiO2 and then AgBr or AgCl particles. Photocatalysts were characterized by using X-ray diffraction, Brunauer–Emmett–Teller (BET), and scanning electron microscopy techniques. Activity was evaluated by photodegradation of Acid Blue 92 as an azo dye. The effect of silver halide deposition on the photocatalytic behavior of the prepared nanocomposites was studied under both ultraviolet (UV) and visible light, and the results were compared. The results showed that AgCl/TiO2/MOR was more active under UV, while with visible source, AgBr/TiO2/MOR exhibited better photocatalytic performance. A mechanism for the reaction is also proposed. 相似文献
Analcime shell-nickel ferrite core microspheres were decorated with Pd and Pt nanoparticles with the aid of an ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate (BMIM-PF6). The samples thus prepared were characterized using X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray (EDX), nitrogen adsorption-desorption isotherms, transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM) methods. The XRD patterns confirmed the growth of a zeolitic layer on the surface of the magnetic cores. The thermogravimetric analysis (TGA) curve clearly indicated the thermal decomposition of the loaded IL, which confirmed the presence of BMIM-PF6 in the structures. In addition, EDX analysis indicated that the samples contained 2.5 mass % of noble metal. The metallic species can be adsorbed on the modified surface and/or penetrate into the zeolitic channels in the structures. The results indicate that the X-IL/An/S/NF (X = Pt or Pd) metallic nanoparticles supported core-shell catalysts-samples were able to catalyse the selective oxidation of cyclohexene to 2-cyclohexene-1-ol under the induced conditions. The catalysts continued to be active after recycling up to 5 times. Eventually, a suitable mechanism was proposed for the selective oxidation of cyclohexene over the catalysts. 相似文献
Structural and molecular-microscopic properties of the solvatochromic probes 4-nitroaniline, 4-nitroanisole, and Reichardt’s dye were investigated in binary mixtures of ethylammonium propionate with methanol, ethanol, 1-propanol and 2-propanol. Solvatochromic parameters (α, hydrogen-bond donor acidity; β, hydrogen-bond acceptor basicity; π*, dipolarity/polarizability; $ E_{\text{T}}^{\text{N}} $, normalized polarity parameter) in different binary mixtures of ionic liquid with molecular solvents were determined with UV–Vis spectroscopy. The $ E_{\text{T}}^{\text{N}} $ parameters show nearly ideal trends in all solvent mixtures, but the other parameters show different behavior in the mixtures. The π* parameters show a negative deviation from ideality in the ionic liquid/methanol system. In contrast, the α parameters have severe positive deviations from ideal behavior in ionic liquid/1-propanol and ionic liquid/2-propanol solvent mixtures. A synergistic solvation effect is observed for the π* parameters in IL/methanol mixtures. Specific solute–solvent interactions or solvent–solvent interactions, which cause non-ideal trends in some parameters, are justified and interpreted by the preferential solvation model. 相似文献
Visible light photoactive silver[orthophosphate-bromide] loaded on fluorapatite (FA) and carboxymethyl cellulose (CMC) supports were prepared by an ionic liquid-assisted precipitation method and used as effective light driven heterogeneous systems for removal of Acid Blue 92 (AB92) azo dye and E. coli gram-negative bacteria from the wastewaters. The prepared samples were characterized by X-ray diffraction (XRD) powder, diffuse reflectance spectroscopy (DRS), Furrier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and nitrogen adsorption-desorption isotherms (BET). The XRD patterns well proved the formation of Ag3PO4 and AgBr photocatalytic crystalline phases of the nanostructures. Besides, the SEM images demonstrated that the photoactive particles were homogenously dispersed on the surface and the average size of the particles is below 90 nm. The antibacterial experiments showed that the products particularly the FA-based photocatalyst can also be utilized as efficient antimicrobial agents. According to the results, the CMC-based photocatalyst was more active during the first time of using while the other one was determined to be promising enough during the recycling tests. 相似文献