Synthesis,Electrochemical and Luminescence Studies of Nickel and Vanadium Complexes Containing Tetradentate Schiff Base Ligand with N2O2 Donor Atoms

A symmetrical tetradentate Schiff base ligand was derived by the condensation of ortho‐vanillin and thiourea in 2:1 molar ratio and adjusted pH. Nickel and vanadyl complexes were obtained using the template method by the reaction of ortho‐vanillin and thiourea with Ni(OAc)₂. 4H₂O and VO(acac)₂ (2:1:1 molar ratio) in absolute ethanol and adjusted pH. The Schiff base ligand and its complexes have been characterized by FT‐IR, ¹H NMR, UV/Vis, elemental analysis and conductometry measurements. In nickel and also vanadyl complexes the ligands were coordinated to the metals via the imine N and enolic O atoms. The complexes have been found to possess 1:1 metal to ligand stoichiometry and the molar conductance data revealed that the metal complexes were non‐electrolytes. The nickel and vanadyl complexes exhibited tetrahedral and square pyramidal coordination geometry, respectively. The emission spectra of the ligand and its complexes were studied in DMSO. Electrochemical properties of the ligand and its complexes were also investigated in the DMF solvent at the 150 mVs^‐1 scan rate. The ligand and its complexes showed irreversible processes at this scan rate.     

Solid-phase extraction of Pb2+ ion from environmental samples onto L-AC-Ag-NP by flame atomic absorption spectrometry (FAAS)

The development of a solid-phase extraction (SPE) procedure for the pre-concentration of trace amounts of Pb²⁺ ion on 2-furan-2-yl-1-furan-2-ylmethyl-1H-benzoimidazole loaded on activated carbon modified with silver nanoparticles (L-AC-Ag-NP) was presented. The metal ion retained on the sorbent was quantitatively determined via complexation with the ligand. The complexed metal ion was efficiently eluted using 10 mL of 4 mol L^?1 sulphuric acid in 10 w/v% acetone. The influences of the analytical parameters, including pH, amounts of the ligand and the solid phase, eluent conditions and sample volume, on the recoveries of the metal ion were optimised. Using the optimised parameters, the linear response of the SPE method for Pb²⁺ ion were in the ranges of 0.2–160 µg L^?1, and the detection limit for Pb²⁺ ion was 0.034 µg L^?1. The proposed method exhibits a pre-concentration factor (PF) of 80 and an enhancement factor of 30 for Pb²⁺ ion. The presented results demonstrate the successful application of the proposed method for the determination of Pb²⁺ ion in some real samples with high recoveries (>93%) and reasonable relative standard deviation (RSD < 2%).     

Synthesis of new water soluble diorganotin(IV) complexes with hydrazones derived from Girard-T reagent as antibacterial and anticancer agents

Three new water-soluble organotin complexes R₂Sn(5-BrSalGT)Cl [R = Ph, Me] and Ph₂Sn(2-OHNaphGT)Cl have been synthesized by the reaction of R₂SnCl₂ (R = Ph or Me) with Schiff bases derived from condensation of Girard-T reagent with 5-bromosalicylaldehyde and 2-naphthaldehyde, (5-BrH₂SalGT)Cl (1) and (2-OHH₂NaphGT)Cl (2). The synthesized compounds have been investigated by elemental analysis, conductometric measurements, IR, ¹H NMR, and ¹¹⁹Sn NMR spectroscopy. These data show that the deporotonated ligand is coordinated to Sn(IV) via ONO atoms and six-coordinate zwitterionic complexes are formed. The ligands and their complexes were investigated for their in vitro toxicity against Gram-positive (Bacillus subtilis and Staphylococcus aureus) and Gram-negative (Escherichia coli and Pseudomonas aeruginosa) bacteria. The results show remarkable antibacterial activity against the studied bacteria. All complexes exhibit more inhibitory effects than the parent ligand. The anticancer activity of all compounds were also performed on HN5 cell line and (2-OHH₂NaphGT)Cl with concentration of 1 mg mL^?1 was found to show higher anticancer activity than other compounds.     

Surfactant effects on the particle size,zeta potential,and stability of starch nanoparticles and their use in a pH-responsive manner

Storage conditions seem to be important in the long-term stability of nanoparticles (NPs). This work studies the effects of surfactants and storage container on particle size distribution and zeta potential during long-term storage of acid hydrolyzed potato starch NPs. The NPs were prepared from potato starch using acid hydrolysis and high-intensity ultrasonication. During the ultrasonic treatment, the surfactants were added dropwise to the solutions to reduce the size and stabilize the formed NPs. Particle size distribution, zeta potential, and FE-SEM were used to characterize the ensuing NPs. Additionally, a 5-month stability study was performed to evaluate the maintenance of potato starch NPs over time at different storage conditions. Then, NPs from corn starch were produced by the same procedure and were used for preparing pH-responsive nanocarriers containing NaHCO₃ for delivery of an anti-cancer drug, FTY720. These NPs were able to release the drug at pH 5.0 because of CO₂ generated from NaHCO₃ in acidic pH and released from the NPs by the production of pores, which accelerate drug release.     

Polythiophene-coated Fe3O4 nanoparticles as a selective adsorbent for magnetic solid-phase extraction of silver(I), gold(III), copper(II) and palladium(II)

We have developed a fast method for sensitive extraction and determination of the metal ions silver(I), gold(III), copper(II) and palladium(II). Fe₃O₄ magnetic nanoparticles were modified with polythiophene and used for extraction the metal ions without a chelating agent. Following extraction, the ions were determined by flow injection inductively coupled plasma optical emission spectrometry. The influence of sample pH, type and volume of eluent, amount of adsorbent, sample volume and time of adsorption and desorption were optimized. Under the optimum conditions, the calibration plots are linear in the 0.75 to 100 μg L^?1 concentration range (R²?>?0.998), limits of detection in the range from 0.2 to 2.0 μg L^?1, and enhancement factors in the range from 70 to 129. Precisions, expressed as relative standard deviations, are lower than 4.2 %. The applicability of the method was demonstrated by the successful analysis of tap water, mineral water, and river water.

Acetone extracted propolis as a novel membrane and its application in phenol biosensors: the case of catechol

A novel biosensor for catechol has been constructed by immobilizing polyphenol oxidase (PPO) into acetone-extracted propolis (AEP) composite modified with gold nanoparticles (GNPs) and attached to multiwalled carbon nanotube (MWCNTs) on a gold electrode surface. The propolis for AEP was obtained from honeybee colonies. Under the optimum conditions, this method could be successfully used for the amperometric determination of catechol within a concentration range of 1 × 10^?6 to 5 × 10^?4?M, with a detection limit of 8 × 10^?7?M (S/N = 3). The effects of pH and operating potential are also explored to optimize the measurement conditions. The best response was obtained at pH?5, while an optimum ratio of signal-to-noise (S/N) was obtained at ?20?mV (versus Ag/AgCl), which was selected as the applied potential for the amperometric measurements. All subsequent experiments were performed at pH?5. Cyclic voltammetry and electrochemical impedance spectroscopy was used to characterize the PPO/CNTs/GNPs/AEP/Au biosensor. The biosensor also exhibited good selectivity, stability, and reproducibility.     

Synthesis of methacrylate derivatives oligomers by dithiobenzoate‐RAFT‐mediated polymerization

Reversible addition fragmentation chain transfer (RAFT) was used to synthesize methacrylic acid oligomers and oligo(methacrylic acid)‐b‐poly(methyl methacrylate) (PMAA‐b‐PMMA) with targeted degree of polymerization ≈ 10. Characterization is by size‐exclusion chromatography (SEC) and electrospray mass‐spectrometry. SEC data are presented as hydrodynamic volume distributions (HVDs), the only proper means to present comparative and meaningful SEC data when there is no unique relationship between size and molecular weight. The RAFT agent, (4‐cyanopentanoic acid)‐4‐dithiobenzoate (CPADB), produced dithiobenzoic acid as a side product during the polymerization of methacrylate derivatives. Precipitation in diethyl ether proved to be an easy way to remove this impurity from the PMAA‐RAFT oligomers. Both unpurified and purified macro‐RAFT agent were used to prepare amphiphilic PMAA‐b‐PMMA copolymers. Diblock copolymer prepared from the purified PMAA homopolymer had a narrower HVD in comparison to those obtained from the equivalent unpurified macro‐RAFT agent. This work shows that while cyanoisopropyl‐dithiobenzoate or CPADB are good RAFT agents for methacrylate derivatives, they exhibit some instability under typical polymerization conditions, and thus when oligomers are targeted, optimal control requires checking for the degradation product and appropriate purification steps when necessary (the same effect is present for larger polymers but is unimportant). © 2008 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 46: 2277–2289, 2008     

The effect of fractional calculus on the formation of quantum-mechanical operators

In this paper, the deformation of the ordinary quantum mechanics is formulated based on the idea of conformable fractional calculus. Some properties of fractional calculus and fractional elementary functions are investigated. The fractional wave equation in 1 + 1 dimension and fractional version of the Lorentz transformation are discussed. Finally, the fractional quantum mechanics is formulated; infinite potential well problem, density of states for the ideal gas, and quantum harmonic oscillator problem are discussed.