Chromium(III), manganese(II) and iron(III) complexes based on hydrazone Schiff-base and azide ligands: synthesis,crystal structure and antimicrobial activity

A tridentate NNO donor hydrazine Schiff base, HL, was obtained from condensation of pyridine 2-carbaldehyde and 4-hydroxy benzohydrazide. HL and azide ligands with Cr(III), Mn(II) and Fe(III) have been used to synthesize [Cr(L)(N₃)(OCH₃)]₂ (1), [Mn(HL)₂(N₃)₂] (2), and [Fe(L)(N₃)(OCH₃)]₂·H₂O (3). HL is quite diverse in its chelating ability and can be a neutral or monoanionic ligand as a tridentate unit. In this paper, we report structures showing different denticities of the ligand having different charges. The ligand 1–3 was characterized by elemental analysis, FT-IR, and UV–vis spectral studies and solid-state structures were determined by single-crystal X-ray diffraction analysis, revealing that 1 and 3 are binuclear, while 2 is mononuclear. The efficiencies of the ligand and the three complexes were evaluated for antimicrobial activity; MIC data revealed that HL 1–3 are not strongly active in comparison to standard drugs.     

Spectrophotometric simultaneous determination of cobalt, copper and nickel using nitroso-R-salt in alloys by partial least squares

Partial least squares modeling as a powerful multivariate statistical tool applied to spectrophotometric simultaneous determination of cobalt, copper, and nickel in aqueous solutions. The concentration range for cobalt, copper and nickel were 0.4-2.6, 0.6-3.4, 0.5-5.5 ppm, respectively. The experimental calibration set was composed with 36 sample solutions using a mixture design for three component mixtures. The absorption spectra were recorded from 470 to 600 nm. The effect of pH on the sensitivity and selectivity was studied according to net analyte signal (NAS). The values of root mean square difference (RMSD) for cobalt, copper and nickel using partial least squares (PLS) were 0.0192, 0.0263 and 0.0446 ppm, respectively. The effects of various cations and anions were investigated. The method was used to determination of cobalt, copper and nickel in two sample alloys based on copper, nickel and cobalt (known as cunico) and based on cobalt, nickel and iron (known as conife).     

A new nano‐sized mononuclear Cu (II) complex with N,N‐donor Schiff base ligands: sonochemical synthesis,characterization, molecular modeling and biological activity

A new, simple Cu²⁺ nano‐structure Schiff base complex in methanol medium has been synthesized by the ultrasonic method. Structure of the compound was confirmed by FT‐IR, GC‐Mass and other spectroscopic techniques. The copper oxide (CuO) was achieved from the copper nano‐structure Schiff base complex as the raw material after calcination for 3 hr at 600 °C. According to results Cu²⁺ gives a complex with mole ratio 1:2 of metal to ligand (ML₂) with Schiff base which a distorted square planer is the most probable geometry for it. The calculations results from XRD patterns propose the nano‐sized complexes. The SEM images show morphology of both the copper complex and the CuO powder were plate‐like. The metal chelates of Cu²⁺ in two states of bulk and nano have been screened for their in vitro antibacterial activity against four bacteria, gram‐positive (Staphylococcus aureus) and gram‐negative (Escherichia coli) and three strains of fungus (Aspergillus flavus). The nano metal chelates were shown to possess more antibacterial activity than the bulk chelate. Finally, the empirical parameters of Schiff base compounds showed a good agreement with theoretical ones.     

Analysis of anatoxin-a using polyaniline as a sorbent in solid-phase microextraction coupled to gas chromatography-mass spectrometry

A simple and sensitive method for determining anatoxin-a in aqueous samples was developed using solid-phase microextraction (SPME) and gas chromatography with mass spectrometry (GC-MS) detection. Three forms of polyaniline (PANI) films and a single form of polypyrrole (PPY) film were prepared and applied for SPME. The extraction properties of these films to anatoxin-a were examined and it was shown that leucoemeraldine form of PANI displayed a better selectivity to this compound. SPME conditions were optimized by selecting the appropriate extraction parameters, including type of coating (leucoemeraldine form of PANI at 32 microm thicknesses), salt concentration (10%, w/v), time of extraction (30 min) and stirring rate (1000 rpm). The calibration curve was linear in the range from 50 to 10,000 ng/ml, with the detection limit (S/N = 3) of 11.2 ng/ml. This method was successfully applied for the analysis of anatoxin-a in the cultured media of two species of cyanobacteria.     

Unique substituted 3-oxo-1,2,3,4-tetrahydropyrazino[1,2-a]benzimidazole-1-carboxamides generated by Ugi 3CC using bifunctional starting material

2-(2-Formyl-1H-benzimidazol-1-yl)acetic acid, as a bifunctional formyl-acid was prepared in four steps. This compound underwent one-pot reaction with primary amines, and alkyl isocyanides under Ugi conditions. A series of novel 3-oxo-1,2,3,4-tetrahydropyrazino[1,2-a]benzimidazole-1-carboxamides were obtained in moderate to excellent yields.     

Preparation of Reinforced poly (BisGMA-UDMA) Graphene-Based Nanocomposites Via Moderate in Situ SET-LRP

In the present study, cross-linked poly (dimethacrylate- urethane dimethacrylate) [poly (BisGMA-UDMA)] functionalized-graphene oxide nanosheets were prepared via single-electron transfer living radical polymerization (SET-LRP) using the ‘grafting from’ strategy, under mild conditions. This method first involves the covalent attachment of Br-containing groups onto the surface of grapheme sheets to give the initiating-groups-containing graphene (G-Br). After that, the succeeding SET-LRP polymerization in DMSO in the presence of a Cu wire/Me₆TREN catalytic system at room temperature leads to the grafting of poly (BisGMA-UDMA) chains onto the graphene surface. The resulting graphene-poly (dimethacrylate- urethane dimethacrylate) (G-PDMA-UDMA) nanocomposites were characterized using FT-IR, XRD, DSC, AFM, FE-SEM, and TEM analysis techniques. It was proved that polymer chains were successfully introduced to the surface of the graphene planes. After grafting with poly (BisGMA-UDMA), the dispersibility of the modified GO sheets significantly improved. When compared to G-PDMA, the resulting G-PDMA-UDMA nanocomposite revealed around 75%, 97%, and 65%, increase in compressive strength, Young's modulus and toughness, respectively. Such smart graphene-based nanocomposites can be used as promising biomaterials in orthopaedic and dental applications with the desired mechanical properties.     

Conjugate Phase Change Heat Transfer in an Inclined Compound Cavity Partially Filled with a Porous Medium: A Deformed Mesh Approach

In this paper, the melting process of a PCM inside an inclined compound enclosure partially filled with a porous medium is theoretically addressed using a novel deformed mesh method. The sub-domain area of the compound enclosure is made of a porous layer and clear region. The right wall of the enclosure is adjacent to the clear region and is subject to a constant temperature of T_c. The left wall, which is connected to the porous layer, is thick and thermally conductive. The thick wall is partially subject to the hot temperature of T_h. The remaining borders of the enclosure are well insulated. The governing equations for flow and heat transfer, including the phase change effects and conjugate heat transfer at the thick wall, are introduced and transformed into a non-dimensional form. A deformed grid method is utilized to track the phase change front in the solid and liquid regions. The melting front movement is controlled by the Stefan condition. The finite element method, along with Arbitrary Eulerian–Lagrangian (ALE) moving grid technique, is employed to solve the non-dimensional governing equations. The modeling approach and the accuracy of the utilized numerical approach are verified by comparison of the results with several experimental and numerical studies, available in the literature. The effect of conjugate wall thickness, inclination angle, and the porous layer thickness on the phase change heat transfer of PCM is investigated. The outcomes show that the rates of melting and heat transfer are enhanced as the thickness of the porous layer increases. The melting rate is the highest when the inclination angle of the enclosure is 45°. An increase in the wall thickness improves the melting rate.

     

Synthesis and anti-brucella activity of some new 1,3,4-oxadiazole derivatives containing a ferrocene unit

An isocyanide-based multicomponent reaction between cinnamic acid derivatives or 3-phenyl-2-propynoic acid, (N-isocyanimino)triphenylphosphorane, ferrocenecarbaldehyde, and dibenzylamine has been reported in excellent yields for the preparation of some new ferrocenyl-containing 1,3,4-oxadiazole derivatives. The anti-brucella activities of the products are investigated in in vitro and in vivo assays.     

Silicon nitride nanoparticles for surface-assisted laser desorption/ionization of small molecules

Conventional matrix-assisted laser desorption/ionization mass spectrometry is limited to analyses of higher molecular weight compounds due to high background noise generated by the matrix in the lower mass region. Surface-assisted laser desorption/ionization (SALDI) mass spectrometry is an alternative solution to this problem. Nanoparticles, structured silicon surfaces and carbon allotropes are commonly used as SALDI surfaces. Here, for the first time, we demonstrate the application of silicon nitride nanoparticles as a suitable medium for laser desorption/ionization of small drug molecules.