Separation of brombuterol enantiomers in capillary electrophoresis with cyclodextrin‐type chiral selectors and investigation of structure of selector‐selectand complexes using nuclear magnetic resonance spectroscopy

The major goal of this study was to determine the affinity pattern of brombuterol (BB) enantiomers toward various cyclodextrins (CD) and to evaluate the potential of NMR spectroscopy for understanding fine mechanisms of interactions between CDs and BB enantiomers. Separation of BB enantiomers was performed in a fused‐silica capillary using a phosphate buffer, pH 2.5, at the room temperature in the normal polarity mode. It was shown once again that CE in combination with NMR spectroscopy represents a very sensitive tool for studies of affinity patterns and structure of CD complexes with chiral guests. Although opposite affinity patterns of BB enantiomers were observed toward native β‐ and γ‐CDs, no significant differences between the structures of the complexes of these two CDs with BB were detected by NMR spectroscopy. In contrary to this, the opposite affinity pattern of BB enantiomers toward β‐CD and its two sulfated derivatives, heptakis (2,3‐O‐diacetyl‐6‐sulfo)‐β‐CD (HDAS‐β‐CD) and heptakis (2‐O‐methyl‐3,6‐di‐O‐sulfo)‐β‐CD (HMDS‐β‐CD) was associated with major differences in the structure of the complexes. In addition, it was shown again that HMDS‐β‐CD provides separation of enantiomers without formation of inclusion‐type complex with the chiral analyte.     

Sensitive Determination of Terbutaline Using a Platform Based on Nanoparticles of Europium Oxide and Carbon Nanotubes

This study presents a sensitive voltammetric determination of terbutaline (TER) on a platform based on carbon nanotubes (CNTs) and europium oxide nanoparticles (Eu₂O₃NPs) coated glassy carbon electrodes (GCEs). An ultrasonic bath was performed for the preparation of composite material. The material was characterized by energy dispersive X‐ray spectroscopy (EDX), X‐ray diffraction method (XRD) and scanning electron microscopy (SEM). The Eu₂O₃NPs/CNTs/GCE system was assessed for the oxidation of terbutaline (TER). A broad oxidation peak was appeared at 0.71 V using a bare GCE. However, the voltammetry of TER has been improved at a GCE coated with CNTs and a well‐defined anodic peak exhibited at 0.61 V. Furthermore, the nanoparticles of Eu₂O₃ and CNTs coated GCE has greatly improved the electrochemical behaviour of TER and a sharp peak was appeared at 0.59 V. Cyclic voltammetry at Eu₂O₃NPs/CNTs/GCE also reveals a high catalytic effect for the oxidation of TER with an oxidation peak that is distinctly enhanced compared to GCE and CNTs/GCE. Eu₂O₃ nanoparticles were utilized to enhance the surface area of GCE and then improve the sensitivity of the procedure. The response of TER was linear over a concentration range of 2.0×10^?8 M ?9.5×10^?6 M with an LOD of 3.7×10^?9 M. Square wave voltammetric analysis of tablets by Eu₂O₃NPs/CNTs/GCE yielded a recovery of 99.2 % with an RSD% of 3.2. The modified electrode (EuO₂NPs/CNTs/GCE) provides accuracy and precision to the analysis of samples.     

Poly(amidoamine) dendrimer‐coated magnetic nanoparticles for the fast purification and selective enrichment of glycopeptides and glycans

Glycosylated proteins modulate various important functions of organisms. To reveal the functions of glycoproteins, in‐depth characterization studies are necessary. Although mass spectrometry is a very efficient tool for glycoproteomic and glycomic studies, efficient sample preparation methods are required prior to analyses. In the study, poly(amidoamine) dendrimer‐coated magnetic nanoparticles were presented for the specific enrichment and fast purification of glycopeptides and glycans. The enrichment and purification performance of the developed method was evaluated both at the glycopeptide, and the glycan level using several standard glycoprotein digests and released glycan samples. The poly(amidoamine) dendrimer‐coated magnetic nanoparticles not only showed selective affinity (Immunoglobulin G/Bovine Serum Albumin, 1/10 by weight) to glycopeptides and released glycans but also good sensitivity (0.4 ng/µL for Immunoglobulin G) for glycoproteomic and glycomic applications. Thirty‐five glycopeptides of Immunoglobulin G were detected after enrichment with poly(amidoamine) dendrimer‐coated magnetic nanoparticles. In addition, 55 ¹⁸O tagged deamidated glycopeptides belonging to human plasma glycoproteome were confirmed. Finally, fifty 2‐aminobenzoic acid, and 30 procainamide‐labelled human plasma N‐glycans released from human plasma glycoproteins were determined after purifications. The results indicate that the proposed enrichment and purification method using poly(amidoamine) dendrimer‐coated magnetic nanoparticles could be simply adjusted to sample preparation methods.     

Exploration of fractal nature of WO3 nanowire aggregates

The morphology of WO₃ aggregates formed by irregular nanoparticles (D∼40 nm) and nanowires of different aspect ratios (2, 4, 6, and 10 μm nominal lengths) dispersed in commonly used polar solvents without dispersant agents is investigated using a small-angle light scattering technique and by means of fractal theory. Nanoparticles form compact spherical aggregates (D_f∼2.6), whereas 2 μm nanowires with low aspect ratio (L/D∼10) follow a slow cluster-cluster aggregation mechanism with no discernable change in fractal dimension (D_f=2.1) monitored in an extended period of 6 months, despite a notable growth in size (R_g=2.3-3.1 μm). For higher aspect ratio nanowires, scattered intensity profiles, which migrate towards the Porod regime, qualitatively obey the Lorenz-Mie theory predictions. The 10 μm nanowires with very high aspect ratio (L/D∼250) are observed to form stable dispersions in a time span of 6 days. Analytical methods based on spherical primary particle formulations predict D_f=1.9, 1.7, and 1.4 for 4, 6, and 10 μm nanowires, respectively.     

Observation of entanglement between two light beams spanning an octave in optical frequency

We have experimentally demonstrated how two beams of light separated by an octave in frequency can become entangled after their interaction in a chi;{(2)} nonlinear medium. The entangler was a nonlinear optical resonator that was strongly driven by coherent light at the fundamental and second-harmonic wavelengths. An interconversion between the fields created quantum correlations in the amplitude and phase quadratures, which were measured by two independent homodyne detectors. Analysis of the resulting correlation matrix revealed a wave function inseparability of 0.74(1)<1, thereby satisfying the criterion of entanglement.     

Current-voltage characteristics of Au/GaN/GaAs structure

Au/GaN/n-GaAs structure has been fabricated by the electrochemically anodic nitridation method for providing an evidence of achievement of stable electronic passivation of n-doped GaAs surface. The change of the electronic properties of the GaAs surface induced by the nitridation process has been studied by means of current-voltage (I-V) characterizations on Schottky barrier diodes (SBDs) shaped on gallium nitride/gallium arsenide structure. Au/GaN/n-GaAs Schottky diode that showed rectifying behavior with an ideality factor value of 2.06 and barrier height value of 0.73 eV obeys a metal-interfacial layer-semiconductor (MIS) configuration rather than an ideal Schottky diode due to the existence of GaN at the Au/GaAs interfacial layer. The formation of the GaN interfacial layer for the stable passivation of gallium arsenide surface is investigated through calculation of the interface state density N_ss with and without taking into account the series resistance R_s. While the interface state density calculated without taking into account R_s has increased exponentially with bias from 2.2×10¹² cm⁻² eV⁻¹ in (E_c−0.48) eV to 3.85×10¹² cm⁻² eV⁻¹ in (E_c−0.32) eV of n-GaAs, the N_ss obtained taking into account the series resistance has remained constant with a value of 2.2×10¹² cm⁻² eV⁻¹ in the same interval. This has been attributed to the passivation of the n-doped GaAs surface with the formation of the GaN interfacial layer.     

Novel impinging jets-based non-periodic sweeping jets

Journal of Visualization -     

N‐Phenyl‐substituted carbene precursors and their silver complexes: synthesis,characterization and antimicrobial activities

A series of unsymmetrically substituted N‐heterocyclic carbene (NHC) precursors ( 1a , 1b , 1c , 1d , 1e ) were synthesized from the reaction of N‐phenylbenzimidazole with various alkyl halides. These compounds were used to synthesize NHC–silver(I) complexes ( 2a , 2b , 2c , 2d , 2e ). The five new 1‐phenyl‐3‐alkylbenzimidazolium salts ( 1a , 1b , 1c , 1d , 1e ) and their NHC–silver complexes ( 2a , 2b , 2c , 2d , 2e ) were characterized by the ¹H NMR, ¹³C NMR and FT‐IR spectroscopic methods and elemental analysis techniques. Also, the two NHC–silver complexes 2b and 2c were characterized by single‐crystal X‐ray crystallography, which confirmed the linear C―Ag―Cl arrangements. The antibacterial activities of the NHC precursor and NHC–silver complexes were tested against three Gram‐positive bacterial strains (Bacillus subtilis, Listeria monocytogenes and Staphylococcus aureus) and three Gram‐negative bacterial strains (Escherichia coli, Klebsiella pneumoniae and Pseudomonas aeruginosa) using the microdilution broth method. The NHC–silver complexes showed higher antibacterial activity than the NHC precursors. In addition, silver complexes 2a , 2b , 2c , 2d showed high antibacterial activity against the Gram‐positive bacteria L. monocytogenes and S. aureus compared to the standard, tetracycline. Copyright © 2014 John Wiley & Sons, Ltd.     

Investigation of 2-aminoethanethiol as corrosion inhibitor for steel using response surface methodology (RSM)

The inhibition efficiency of 2-aminoethanethiol (2-AEE) has been investigated against steel corrosion in 0.1 M HCl solution. The effect of temperature, pH, and concentration were studied with the help of potentiodynamic measurement, electrochemical impedance spectroscopy, scanning electron microscopy, and atomic absorption spectroscopy techniques. The potential of zero charge (E_pzc) studies showed that the adsorption occurs via ?SH group; the metal surface is positively charged in corrosive test solution. The adsorptive interaction is evaluated, and best correlation was obtained with Langmuir isotherm. 2-AEE was shown to have significant inhibition efficiency against steel corrosion. The response surface methodology was employed to explain the relation between pH, inhibitor concentration, and the efficiency. The regression analysis was realized for development of an equation between independent variables and the output. The success of fitting model was tested with basic statistical arguments, residual and variance analysis, T and F tests, and R ² value. The statistical evaluations showed that the obtained polynomial equation can be successfully used for optimization of applications involving the use of 2-AEE as inhibitor.     

Spectroscopic and theoretical optical properties of indoleninyl-substituted dibenzotetraaza[14]annulenes

Two new macrocyclic dibenzotetraaza[14]annulene (DBTAA) compounds with indolenine ( 5 ) and pyridoindolenine ( 6 ) moieties were synthesized and characterized by spectroscopy. Both DBTAAs exhibit strong UV-Vis absorption properties in the Soret band region. The theoretical second-order nonlinear optical property, electric dipole moment (μ), dispersion-free dipole polarizability (α) and first hyper-polarizability values were calculated by density functional theory and time dependent density functional theory. The ab-initio quantum mechanical calculation by time-dependent Hartree-Fock method was utilized to investigate the dynamic dipole polarizabilities, dynamic second-order, static, and dynamic third-order (γ) hyper-polarizabilities of the DBTAAs. The configuration interaction technique of all doubly occupied molecular orbitals possesses theoretically defined single-photon absorption (OPA) specifications for the examined structures. The computed maximum OPA wavelengths on both macrocyclic compounds coincide with the preceding measurement outcomes.