Preparation,heat treatment and photoluminescence properties of V-doped ZnO–SiO2–B2O3 glasses

Four glasses in ZnO–SiO₂–B₂O₃ ternary system were prepared by the melt quenching method with the objective of optimizing sub-nanosecond emission over the UV region of zinc borosilicate glasses used in superfast scintillators. The effect of vanadium addition and heat treatment on phase formation, microstructure and photoluminescence properties of the glasses was characterized by means of DTA, XRD, SEM and fluorescence spectrophotometer. Vanadium contributed to the near-band-edge emission in two ways, by introducing donor levels in the energy band of ZnO particles and by facilitating the precipitation of ZnO and willemite crystals. Furthermore, nucleation of willemite and zinc oxide phases, which are both the origins of the intense emission bands in the UV region, was facilitated with increasing either the time or temperature of heat treatments. Photoluminescence spectra showed the elimination of the visible emission band which is favorable in scintillating glasses.     

Click synthesis of 1,4-disubstituted-1,2,3-triazoles catalyzed by melamine-supported CuO nanoparticles as an efficient recyclable catalyst in water

Melamine-supported CuO nanoparticles (M-CuO nanocatalyst) are prepared as a new and efficient recyclable nanocatalyst for the regioselective synthesis of 1,2,3-triazoles in water. This new nanocatalyst was prepared by co-precipitation method and characterized by FT-IR spectral study, TGA, DSC, XRF, ICP-OES, XRD, SEM, EDS and BET analysis. A wide range of 1,4-disubstituted-1,2,3-triazoles were synthesized from reaction of benzyl halides or alkyl halides with phenyl acetylene and sodium azide in high yields. M-CuO nanocatalyst could be reused more than 6 times without considerable loss of its initial activity.

     

Convenient regioselective reaction in presence of H<Subscript>3</Subscript>PW<Subscript>12</Subscript>O<Subscript>40</Subscript>: synthesis and characterization of pyrazolo[3,4-<Emphasis Type="Italic">b</Emphasis>]quinoline-3,5-diones

We describe regioselective synthesis of pyrazolo[3,4-b]quinoline derivatives by multicomponent reaction of dimedone, 5-aminopyrazolone, and aromatic aldehydes in presence of H₃PW₁₂O₄₀ as catalyst. When this multicomponent reaction was investigated without catalyst under reflux conditions, a mixture of products was obtained, while the reaction successfully proceeded to formation of pyrazolo[3,4-b]quinoline in presence of H₃PW₁₂O₄₀. Good product yield, short experimental time, and low-cost catalyst provide convenient synthesis for formation of pyrazolo[3,4-b]quinoline pharmacological compounds.     

Hydrophobic Deep Eutectic Solvents in Developing Microextraction Methods Based on Solidification of Floating Drop: Application to the Trace HPLC/FLD Determination of PAHs

In this work, we evaluated the applicability of hydrophobic carboxylic acid-based deep eutectic solvents (DESs) as environmentally friendly alternatives to common organic solvents in microextraction methods based on solidification of floating drop (SFD). Due to the limited number of solvents that can be used in SFD, the introduction of new solvents can help in the development of these attractive methods. Deep eutectic solvents consisting of tetra-n-butyl ammonium bromide (TBAB) and carboxylic acids were prepared and used as extraction solvent. They had the desirable characteristics such as low density, suitable freezing point and proper hydrophobicity which make them suitable alternatives to conventional organic solvents for SFD. With the help of the synthesized hydrophobic DESs, a simple, fast, efficient and environmentally friendly microextraction method was developed based on solidification of deep eutectic solvent (SFDES) without using any organic solvent. The proposed organic solvent-less microextraction method based on SFDES was applied in the analysis of polycyclic aromatic hydrocarbons (PAHs) as model compounds in environmental water samples. By coupling this method with high-performance liquid chromatography–fluorescence detection, we achieved low LOD values which is a necessity in the ultra-trace analysis of PAHs in environmental water samples. Under the optimized conditions, good linearity and low limits of detection of 0.7–6.6 ng L^?1 were obtained. The analysis of six PAHs in real water samples gave acceptable relative recoveries ranging from 83 to 117% with 5.4–10.5% intra-day relative standard deviations (RSD) and 4–7.1% interday RSD.

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Development of capillary zone electrophoresis-electrospray ionization-mass spectrometry for the determination of lamotrigine in human plasma

A method of coupling capillary zone electrophoresis (CZE) with electrospray ionization-mass spectrometry (ESI-MS) detection has been developed for monitoring an antiepileptic drug, lamotrigine (LTG) in human plasma. The CZE-MS was developed in three stages: (i) CZE separation and ESI-MS detection of LTG and tyramine (TRM, internal standard) were simultaneously optimized by studying the influence of CZE background electrolyte (BGE) pH, BGE ionic strength, and nebulizer pressure of the MS sprayer; (ii) sheath liquid parameters, such as pH, ionic strength, organic modifier content, and flow rate of the sheath liquid, were systematically varied under optimum CZE-MS conditions developed in the first stage; (iii) MS sprayer chamber parameters (drying gas temperature and drying gas flow rate) were varied for the best MS detection of LTG. The developed assay was finally applied for the determination of LTG in plasma samples. The linear range of LTG in plasma sample assay was between 0.1-5.0 microg/mL with a limit of detection as low as 0.05 microg/mL and run time less than 6 min. Finally, the concentration-time profile of LTG in human plasma sample was found to correlate well when CZE-ESI-MS was compared to a more established method of high-performance liquid chromatography with ultraviolet detection.     

Chiral separations in microemulsion electrokinetic chromatography. Use of micelle polymers and microemulsion polymers

In this study, microemulsions of the chiral surfactant polysodium N-undecenoyl-D-valinate (poly-D-SUV) was utilized for enantiomeric separation by investigating two approaches using polymeric chiral surfactant in microemulsion electrokinetic chromatography (MEEKC). In the first approach, poly-D-SUV was used as an emulsifier surfactant along with 1-butanol and n-heptane. Enantioseparation of anionic or partially anionic binaphthyl derivatives, anionic barbiturates, and cationic paveroline derivatives were achieved by varying the mass fraction of 1-butanol, n-heptane and poly-D-SUV. For anionic or partially anionic analytes, relatively lower mass fractions of n-heptane, and poly-D-SUV were found to give optimum chiral separations as compared to that for cationic solutes. In the second approach, the chiral microemulsion polymer was prepared by polymerizing mixtures of 3.50% (w/w) of sodium N-undecenoyl-D-valinate (D-SUV) and 0.82% (w/w) of n-heptane (core phase) at varying concentration of 1-butanol. After polymerization, the n-heptane and 1-butanol were removed to yield solvent free microemulsion polymers (MPs) which were then utilized for the separation of anionic binaphthyl derivatives and anionic barbiturates. When MPs of D-SUV were utilized for chiral separation, 1.00% (w/w) 1-butanol and 3.50% (w/w) 1-butanol was optimum for enantioseparation of (+/-)-BNP and (+/-)-BOH, respectively. On the other hand, for anionic (+/-)-barbiturates very low concentration of butanol (0.25%, w/w) provided optimum resolution. Compared with micellar electrokinetic chromatography (MEKC), the use of micelle polymers or microemulsion polymers in MEEKC showed dramatic enhancement for resolution of (+/-)-BNP, while this enhancement was less dramatic for other binaphthyls [(+/-)-BOH, (+/-)-BNA] as well as for (+/-)-barbiturates and (+/-)-paveroline derivatives. However, higher separation efficiency of the enantiomers was always observed with MEEKC than in MEKC.     

Preparation and characterization of MNPs–PhSO3H as a heterogeneous catalyst for the synthesis of benzo[b]pyran and pyrano[3,2-c]chromenes

Research on Chemical Intermediates - In this study, an efficient and novel procedure has been reported for loading sulfanilic acid on the surface of magnetite Fe3O4 nanoparticles using...