Eco‐friendly ionic liquid assisted capillary electrophoresis and α‐acid glycoprotein‐assisted liquid chromatography for simultaneous determination of anticancer drugs in human fluids

In the current work, two eco‐friendly analytical methods based on capillary electrophoresis (CE) and reversed phase liquid chromatography (RPLC) were developed for simultaneous determination of the most commonly used anticancer drugs for Hodgkin's disease: methotrexate (MTX), vinblastine, chlorambucil and dacarbazine. A background electrolyte (BGE) of 12.5 mmol/L phosphate buffer at pH 7.4 and 0.1 µmol/L 1‐butyl‐3‐methyl imidazolium bromide (BMImBr) ionic liquid (IL) was used for CE measurements at 250 nm detection wavelength, 20 kV applied voltage and 25 °C. The rinsing protocol was significantly improved to reduce the adsorption of IL on the interior surface of capillary. Moreover, RPLC method was developed on α‐1‐acid glycoprotein (AGP) column. Mobile phase was 10 mmol/L phosphate buffer at pH 6.0 (100% v/v) and flow rate at 0.1 mL/min. As AGP is a chiral column, it was successfully separated l ‐MTX from its enantiomer impurity d ‐MTX. Good linearity of quantitative analysis was achieved with coefficients of determinations (r²) >0.995. The stability of drugs measurements was investigated with adequate recoveries up to 24 h storage time under ambient temperature. The limits of detection were <50 and 90 ng/mL by CE and RPLC, respectively. The using of short‐chain IL as an additive in BGE achieved 600‐fold sensitivity enhancement compared with conventional Capillary Zone Electrophoresis (CZE). Therefore, for the first time, the proposed methods were successfully applied to determine simultaneously the analytes in human plasma and urine samples at clinically relevant concentrations with fast and simple pretreatments. Developed IL‐assisted CE and RPLC methods were also applied to measure MTX levels in patients’ samples over time. Copyright © 2014 John Wiley & Sons, Ltd.     

Study of thermal currents in powder β-spodumene ceramics doped with Cuo, FeO and TiO2

Ternary-phase ceramic system of Li₂O Al₂O₃ 4SiO₂ doped with CuO, FeO and TiO₂ has been prepared and subjected to dc electrical conductivity and thermally stimulated depolarization current (TSDC) measurements as a function of temperature (30-250 °C) and field strength. The electrical conductivity results are explained by assuming both ionic and electronic conduction mechanisms coexist with different contributions over the whole temperature range of experiments. TSDC spectra have been found to be characterized by a broad intense relaxation peak, which can be attributed to an ionic charge polarization. The broad relaxation transitions are apparently a result of the nonuniform nature of this process. Activation energies are calculated for both dc electrical conductivity and TSDC according to Arrhenius equation and initial rise method, respectively.     

Pre—Separation Axioms in Fuzzifying Topology

1　 IntroductionYing[5,6 ] introduced and elementally developed so called fuzzifying topology with the semanticmethod of continuous valued L ogic.Shen[7] introduced and studied T0 -,T1-,T2 (Hausdorff) -,T3(regularity) -,T4 (normality) -separation axioms in fuzzifying topology.In [3 ]the concepts of thefamily of fuzzifying pre-open sets,fuzzifying pre-neighbourhood structure of a point and fuzzifyingpre-closure are introduced and studied.It is worth to mention that pre-separation axioms are …     

Nonlinear electrohydrodynamic instability of a finitely conducting cylinder: Effect of interfacial surface charges

The nonlinear electrohydrodynamic stability of cylindrical interface, supporting surface charge, among two conducting fluids is investigated. The two fluids are subjected to a radial electric field. The analysis based on the multiple scale technique. It is shown that the evolution of the amplitude is governed by two partial differential equations. These equations are combined to yield two alternate Schrödinger equations with cubic nonlinearity. One of which calculates the nonlinear cutoff electric field, separating stable and unstable disturbances, while the other is used to analyze the stability of the system. The stability criteria are analytically discussed and numerically confirmed. Numerical calculations resulted in set of graphs to indicate the stability picture of the considered system.     

在重力场和磁场影响下自旋刚性航天器的周期运动

考虑重力场和磁场对轴对称航天器本体的影响，研究其质心在圆形轨道上的运动,通过降低系统的运动方程数，并将它变成为一个带电粒子在电磁场作用下的平面运动．确认系统运动是稳定的，并通过Liapunov全纯积分定理，构建其近似的周期运动.     

Structural and electrical characterization of SxSe100−x thin films

Thin films of samples of the glassy S_xSe_100−x system with 0 ≤ x ≤ 7.28 have been prepared by thermal evaporation technique at room temperature (300 K). X-ray investigations show that the structure of pure selenium (Se) does change seriously by the addition of small amount of sulphur S ≤7.28%. The lattice parameters were determined as a function of sulphur content. Results of differential thermal analysis (DTA) of the glassy compositions of the system S_xSe_100−x were discussed. The characteristic temperatures (T_g, T_c and T_m) were evaluated. Dark electrical resistivities, ρ, of S_xSe_100−x thin films with different thicknesses from 100 to 500 nm, were measured in the temperature range from 300 to 423 K. Two distinct linear parts with different activation energies were observed. The variation of electrical resistivity of examined compositions has been discussed as a function of the film thickness, temperature and the sulphur content. The application of Mott model for the phonon assisted hopping of small polarons gave the same two activation energies obtained from the resistivity temperature calculations.     

Development of the FTIR properties of nano-structure silica gel doped with different rare earth elements,prepared by sol-gel route

Structural characteristics of pure silica gel (silica-xerogel, SiO₂) and silica gel doped with some rare earth elements (REEs) such as, praseodymium Pr³⁺, and Europium Eu³⁺, Erbium Er³⁺ and Holmium Ho³⁺ ions, with different concentrations ranging from 1 up to 6%, in the form of monolith materials were prepared by sol-gel technique, Using tetra-ethoxysilane as precursor materials, which are of particular interest for sol-gel integrated optics applications. Some structural features of sol-gel derived monolith are analyzed, namely the structure of nano-particle momolith samples, based on X-ray diffraction (XRD) and Fourier Transform Infrared (FTIR). We show that the XRD spectra of α-crystobalite are obtained for the pure samples at 1100°C and even by doping with the four REEs ions.     

Laser spectroscopic investigation of salicylic acids hydrogen bonded with water in supersonic jets: Microsolvation effects for excited state proton dislocation

Geometric structures and excited-state proton dislocation of size-selected salicylic acid clusters (salicylic acid and 5-methoxysalicylic acid) with water were studied by using laser spectroscopic techniques. Fluorescence excitation, dispersed fluorescence, and infrared (IR) spectra of those clusters in supersonic jets were examined for both the electronic ground (S0) and first excited (S1) states. The geometric structures of the clusters were determined on the basis of the IR spectra of the OH stretch region with the help of quantum chemical calculations. The hydroxyl group of the water moiety in the clusters forms a ring involving the carboxylic group of the salicylic acid moiety. The IR spectra in S0 show that the intramolecular hydrogen bond in the salicylic acid moiety is still held upon cluster formation, but the phenolic OH stretch band intensity is remarkably weaken in the clusters. The IR spectra in the S1 state and dispersed fluorescence spectra indicated that the intramolecular excited state proton dislocation is hardly affected by the microsolvation with water, in contrast with the strong suppression of the dislocation in the self-solvation.     

Synthesis and Preliminary Anti‐bacterial Activity of Some 4‐Substituted‐N1‐2‐pyridylsulfanilamide Derivatives

2‐Amino‐4‐ethoxycarbonylpyridine 1 was used as a starting material in the synthesis of some 4‐substituted‐N¹‐2‐pyridylsulfanilamide derivatives to evaluate their antimicrobial activity. The obtained compounds were of no particular effect against the tested organisms except for a noticeable inhibition of B. subtilis, which was of varying extents but remained clearly significant.     

Synthesis,characterization and biomimetic oxygenations of manganese(II), iron(III) and copper(II) pyridyl hydrazone complexes

The preparation and characterization of MnII, FeIII and CuII complexes of three tridentate pyridyl hydrazones are reported. The ligands were prepared via Schiff base condensation of 6-chloro-2-hydrazopyridine with alpha-formyl-(L1), alpha-acetyl-(L2), or alpha-benzoyl-(L3) pyridine. The structural characterization of the compounds prepared was based on elemental analyses, electrical conductance and magnetic moment measurements, 1H-n.m.r., i.r., u.v.-vis. and e.s.r spectroscopic methods. The overall structure and reactivity of the metal chelates critically depend on the ligand substituents within the carbonyl moiety. Octahedral and tetrahedral monomeric species were proposed for MnII complexes, and an octahedral environment for the FeIII complexes. Regarding the copper(II) complexes, a monomeric square-planar and a dimeric structure with a chloride bridge in square-pyramidal geometry were suggested. In the presence of molecular oxygen, MnII and CuII complexes catalyse the oxidative transformation of catechol (benzene-1,2-diol) to the corresponding o-benzoquinone. Iron(III) complexes catalyse the aerobic oxidation of catechol to the intradiol cleavage product. The catalytic activity has been correlated with the Lewis acidity of the metal centres created according to the nature of the ligand substituents. The probable mechanistic implications of the catalysed oxidation reactions are discussed. This revised version was published online in June 2006 with corrections to the Cover Date.