Reversed-phase dispersive liquid-liquid microextraction with central composite design optimization for preconcentration and HPLC determination of oleuropein

A reversed-phase dispersive liquid-liquid microextraction (RP-DLLME) method was developed for the preconcentration and direct HPLC determination of oleuropein in olive's processing wastewater (OPW) and olive leaves extracts. In conventional DLLME, the sedimented phase is a micro-drop of a chlorinated organic solvent that is not compatible with RP-HPLC. Therefore, solvent evaporation and reconstitution with an appropriate solvent is often required. In RP-DLLME, this problem was overcome by overturning the solvent polarity in the ordinary DLLME and replacing the organic solvent with water. A central composite chemometrics design was used for multivariate optimization of the effects of five different parameters influencing the extraction efficiency of the method. In the optimized conditions, a mixture of 1.4 mL of an ethyl acetate extract of sample and 40 μL water (pH 5.0) was rapidly injected into 5.3 mL of cyclohexane. After centrifugation of the formed cloudy mixture, a micro-drop of the aqueous phase was sedimented at the conical bottom of the centrifuge tube. This phase, that contained the preconcentrated and partially purified analyte, was directly injected into an RP-HPLC column for analysis. A mean extraction recovery of 102.5 (±4.5) % with enrichment factors exceeding 38, was obtained for five replicated analysis. The detection limit of the method (3σ) for OE was 0.02 μg L⁻¹ for OPW and 2 × 10⁻³ mg kg⁻¹ for olive leaves samples. The results showed that, RP-DLLME is a promising technique which is quick, easily operated and can be directly coupled to HPLC.     

Simultaneous Determination of Ultra Trace of Uranium and Cadmium by Adsorptive Cathodic Stripping Voltammetry Using H‐Point Standard Addition Method

A sensitive adsorptive cathodic stripping voltammetry with H‐point standard addition method for simultaneous determination of uranium and cadmium has been developed. The trace amounts of these metal ions can be simultaneously determined using the Levodpa as complexing agent. Optimal conditions were: accumulation time 50 s, accumulation potential 0.0 mV, scan rate 40 mV s^?1, supporting electrolyte 0.1 M ammonium buffer pH 9.6, and 1×10^?5 M of Levodopa. The results revealed that the cadmium and uranium could be simultaneously determined by H‐point standard addition method with different concentration ratios of uranium to cadmium. The method was successfully applied in a several of real samples.     

Methyl Methacrylate–Ethyleneglycol Dimethacrylate–Acrylic Acid Surface as Stationary Phase for Stir Bar Sorptive Extraction

A novel poly(methyl methacrylate–ethyleneglycol dimethacrylate–acrylic acid) film has been introduced for coating on stir bars to sorptive extraction (SBSE). The effects of different contents of porogen, monomer, cross-linker, modifier and initiator during the solvent or bulk polymerization step on the mechanical property and solvent resistant of prepared sorptive stir bars were investigated. The evaluation of results were caused to obtain the four prepared sorptive stir bars with good mechanical stability and excellent resistance to organic solvents. The extraction efficiency of these prepared sorptive stir bars were investigated by liquid desorption-liquid chromatography-ultraviolet detection (LD-LC-UV) using N-Nitrosodiphenylamine as target analyte. SBSE assays showed the sorptive stir bar that prepared using solution polymerization method had the better recovery for N-Nitrosodiphenylamine in water samples. This sorptive stir bar showed good linearity and acceptable recoveries, as well as advantages such as sensitivity, simplicity, low cost and high feasibility. Based on atomic force microscopy (AFM) results, the average pore size of optimum prepared stir bar using solvent polymerization method was obtained ~9 nm. The thermal gravity (TG) and differential scanning calorimetric (DSC) results showed this polyacrylate film has high thermal stability.     

Nano-sized Cu6Sn5 alloy prepared by a co-precipitation reductive route

Nano-sized Cu₆Sn₅ alloy powders were prepared by a co-precipitation reductive route using a hydrothermal method at 80 °C. The nano-size and morphology of the synthesized Cu₆Sn₅ alloy powders were evaluated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The obtained morphologies, chemical compositions are comparatively discussed. A variety of synthesis parameters, such as time, capping agent and sort of reductant, has an effect on the morphology of the obtained materials, and will be particularly highlighted.     

Involutions on certain Banach algebras related to locally compact groups

Let \(\mathcal{{A}}\) be a Banach algebra and let \(\mathcal{{X}}\) be an introverted closed subspace of \(\mathcal{{A}}^*\) . Here, we give necessary and sufficient conditions for that the dual algebra \(\mathcal{{X}}^*\) of \(\mathcal{{X}}\) or the topological centers \({\mathfrak {Z}}_t^{(1)}(\mathcal{{X}}^{*})\) and \({\mathfrak {Z}}_t^{(2)}(\mathcal{{X}}^{*})\) of \(\mathcal{{X}}^*\) are Banach \(*\) -algebras. We finally apply these results to the Banach space \(L_0^\infty (G)\) of all equivalence classes of essentially bounded functions vanishing at infinity on a locally compact group \(G\) .     

Synthesis of a new palladium salt using N‐benzyl DABCO chloride and its application in Suzuki reaction

A palladium catalyst was synthesized using N‐benzyl DABCO chloride and palladium chloride. The structure of this catalyst was characterized and then the catalyst was used in Suzuki cross‐ coupling reaction of different aryl halides with arylboronic acids. All substrates afforded the corresponding products in good to high yields in the presence of low amounts of the catalyst. Under the heating conditions employed, cheaper and more available aryl chlorides gave relatively high yields in the Suzuki reaction. Copyright © 2012 John Wiley & Sons, Ltd.     

Palladium nanoparticles immobilized on sepiolite–cyclodextrin nanosponge hybrid: Efficient heterogeneous catalyst for ligand‐ and copper‐free C─C coupling reactions

A novel hybrid system composed of sepiolite clay and cyclodextrin nanosponge (CDNS) was prepared via reaction of Cl‐functionalized sepiolite with amine‐functionalized CDNS. CDNS–sepiolite was then applied for immobilization of Pd(0) nanoparticles. The resulting hybrid system, Pd@CDNS‐sepiolite, was characterized using various techniques and successfully used as an efficient and heterogeneous catalyst for ligand‐ and copper‐free Sonogashira and Heck coupling reactions under mild reaction conditions. Recycling experiments confirmed that Pd@CDNS‐sepiolite was recyclable and could be used for several consecutive reaction runs with slight Pd leaching and loss of catalytic activity.     

Dimeric ortho‐palladated homoveratrylamine as an efficient homogeneous catalyst for copper‐free Sonogashira cross‐coupling reaction

The catalytic activity of ortho‐palladated [Pd{C6H2(CH2CH2NH2)‐(OMe)2,3,4}(m‐Br)]2, a complex of homoveratrylamine in the copper‐free Sonogashira coupling reaction has been investigated. This complex is a catalyst that is efficient, stable and non‐sensitive to air and moisture in the Sonogashira reaction. In this homogeneous catalytic system, various aryl halides were efficiently coupled with phenylacetylene in mostly moderate to good yields in N‐methylpyrrolidone at 100 °C under copper‐free conditions. Copyright © 2012 John Wiley & Sons, Ltd.     

One-pot Synthesis of 3-Aminoimidazo[1,2-a]pyridines Catalyzed by Heteropolyacids

Condensation of aldehydes, isonitriles and 2‐aminopyridines in the presence of H₃PMo₁₂O₄₀ affords different derivatives of 3‐aminoimidazo[1,2‐a]pyridine in good to excellent yields.