HPLC column-switching technique for sample preparation and fluorescence determination of propranolol in urine using fused-core columns in both dimensions

A new and fast high-performance liquid chromatography (HPLC) column-switching method using fused-core columns in both dimensions for sample preconcentration and determination of propranolol in human urine has been developed. On-line sample pretreatment and propranolol preconcentration were performed on an Ascentis Express RP-C-18 guard column (5?×?4.6 mm), particle size, 2.7 μm, with mobile phase acetonitrile/water (5:95, v/v) at a flow rate of 2.0 mL min^?1 and at a temperature of 50 °C. Valve switch from pretreatment column to analytical column was set at 4.0 min in a back-flush mode. Separation of propranolol from other endogenous urine compounds was achieved on the fused-core column Ascentis Express RP-Amide (100?×?4.6 mm), particle size, 2.7 μm, with mobile phase acetonitrile/water solution of 0.5 % triethylamine, pH adjusted to 4.5 by means of glacial acetic acid (25:75, v/v), at a flow rate of 1.0 mL min^?1 and at a temperature of 50 °C. Fluorescence excitation/emission detection wavelengths were set at 229/338 nm. A volume of 1,500 μL of filtered urine sample solution was injected directly into the column-switching HPLC system. The total analysis time including on-line sample pretreatment was less than 8 min. The experimentally determined limit of detection of the method was found to be 0.015 ng mL^?1.

Sulphur distribution in the products of waste tire pyrolysis

The aim of the presented work was to investigate the distribution of sulphur in tire pyrolysis products as well as the influence of process parameters (temperature and residence time) on sulphur distribution due to environmental concerns. Among modern methods used for waste tire recycling, pyrolysis is one of the most reasonable alternatives meeting current environmental standards. However, waste tire sulphur content can be a potential drawback for pyrolysis products utilisation as fuels. Sulphur is present in tires in different concentrations, depending on the type and age of the tires. Typical sulphur content in tires is about 1.6 mass %. In this paper, the distribution of sulphur in tire pyrolysis products was investigated. Tire pyrolysis yields three different products: liquid, gaseous, and solid residue composed mostly of carbon black (chars). Temperature and residence time are the two most important parameters affecting the yield and composition of the volatile fraction and they are therefore expected to affect the sulphur content in residues. Pyrolysis experiments were carried out in a laboratory pyrolysis reaction unit in the temperature range of 650°C to 750°C at different residence times: 88.6 s, 80.2 s, and 73.9 s. Liquid and solid products were analysed by elemental analysis and the distribution of total sulphur in tire pyrolysis products was calculated.     

Application of Novel Zn‐Ferrite Modified Glassy Carbon Paste Electrode as a Sensor for Determination of Cd(II) in Waste Water

This paper describes the preparation of a new sensor based on Zn‐ferrite modified glassy carbon paste electrode and its electrochemical application for the determination of trace Cd(II) ions in waste waters using differential pulse anodic stripping voltammetry (DPASV). Different Zn/Ni ferrite nanoparticles were synthesized and characterized using scanning electron microscopy (SEM) and X‐ray powder diffraction (XRPD). The prepared ferrite nanoparticles were used for the preparation of Zn‐ferrite‐modified glassy carbon paste electrode (ZnMGCPE) for determination of Cd(II) at nanomolar levels in waste water at pH 5. The different parameters such as conditions of preparation, Zn²⁺/Ni²⁺/Fe²⁺ ratio and electrochemical parameters, percentage of modifier, accumulation time, pH and accumulation potential were investigated. Besides, interference measurements were also evaluated under optimized parameters. The best voltammetric response was observed for ZnFe₂O₄ modifier, when the percentage of modifier was 3 %, accumulation time 9 min, pH of supporting electrolyte 5 and accumulation potential ?1.05 V. Thus prepared electrode displays excellent response to Cd(II) with a detection limit of 0.38 ppb, and selective detection toward Cd(II) was achieved.     

One-phase supported titanium-based catalyst for polymerization of ethylene. IV. Effect of alkyl group at organoaluminium compound on catalyst performance

The effect of a basic layer (SiO₂—R₃Al intermediate) in the one-phase silica supported titanium-based catalyst was investigated using the simple model catalyst systems obtained by reacting the activated silica gel consecutively with R₃Al and TiCl₄. Mode of the interaction of SiO₂ with R₃Al—resulting in the formation of the basic layer—was observed via analysis of the concentration of the unreacted OH groups on the silica surface employing IR spectroscopy and via analysis of the concentration of aluminium in solvent using AA spectroscopy. It was found that nature of the alkyl group in R₃Al modified the structure of the basic layer, thus influencing the catalyst performance including the concentration of both the sum of Ti²⁺ and Ti³⁺ and the ESR-active Ti (III) centers. The sum of Ti²⁺ and Ti³⁺ ranged from 45 to 52 mol % and the amount of the ESR-active Ti (III) species ranged from 6 to 17 mol % of the all titanium content. A significant effect of alkyl group at organoaluminium compound on the molecular weight distribution of the resulting polymer was observed. © 1996 John Wiley & Sons, Inc.     

Iboga Inspired N-Indolylethyl-Substituted Isoquinuclidines as a Bioactive Scaffold: Chemoenzymatic Synthesis and Characterization as GDNF Releasers and Antitrypanosoma Agents

The first stage of the drug discovery process involves the identification of small compounds with biological activity. Iboga alkaloids are monoterpene indole alkaloids (MIAs) containing a fused isoquinuclidine-tetrahydroazepine ring. Both the natural products and the iboga-inspired synthetic analogs have shown a wide variety of biological activities. Herein, we describe the chemoenzymatic preparation of a small library of novel N-indolylethyl-substituted isoquinuclidines as iboga-inspired compounds, using toluene as a starting material and an imine Diels–Alder reaction as the key step in the synthesis. The new iboga series was investigated for its potential to promote the release of glial cell line-derived neurotrophic factor (GDNF) by C6 glioma cells, and to inhibit the growth of infective trypanosomes. GDNF is a neurotrophic factor widely recognized by its crucial role in development, survival, maintenance, and protection of dopaminergic neuronal circuitries affected in several neurological and psychiatric pathologies. Four compounds of the series showed promising activity as GDNF releasers, and a leading structure (compound 11) was identified for further studies. The same four compounds impaired the growth of bloodstream Trypanosoma brucei brucei (EC₅₀ 1–8 μM) and two of them (compounds 6 and 14) showed a good selectivity index.     

Factorizations of complete graphs into caterpillars of diameter 5

We examine factorizations of complete graphs K_2n into caterpillars of diameter 5. First we present a construction generalizing some previously known methods. Then we use the new method along with some previous partial results to give a complete characterization of caterpillars of diameter 5, which factorize the complete graph K_2n.     

Quantum electrodynamics for vector mesons

Quantum electrodynamics for rho mesons is considered. It is shown that, at the tree level, the value of the gyromagnetic ratio of the rho+ is fixed to 2 in a self-consistent effective quantum field theory. Further, the mixing parameter of the photon and the neutral vector meson is equal to the ratio of electromagnetic and strong couplings, leading to the mass difference M(rho0)-M(rho+/-) approximately 1 MeV at tree order.     

Improving detector signal processing with pulse height analysis in Mössbauer spectrometers

A plenty of different programming techniques and instrument solutions are used in the development of Mössbauer spectrometers. Each of them should provide a faster spectrum accumulation process, increased productivity of measurements, decreased nonlinearity of the velocity scale, etc. The well known virtual instrumentation programming method has been used to design a computer-based Mössbauer spectrometer. Hardware solution was based on two commercially-available PCI modules produced by National Instruments Co. Virtual Mössbauer spectrometer is implemented by the graphical programming language LabVIEW 7 Express. This design environment allows to emulate the multichannel analyzer on the digital oscilloscope platform. This is a novel method based on Waveform Peak Detection function which allows detailed analysis of the acquired signal. The optimal treatment of the detector signal from various detector types is achieved by mathematical processing only. As a result, the possibility of an increase of signal/noise ratio is presented.     

Birefringence dispersion in a quartz crystal retrieved from a channeled spectrum resolved by a fiber-optic spectrometer

We present a simple method for measuring the wavelength dependence of both the phase and group birefringences in a quartz crystal of known thickness. The method utilizes interference of polarized waves resolved by a fiber-optic spectrometer as a channeled spectrum (spectral fringes). The fringe order versus the precise position of the interference maximum in the spectrum is fitted to the approximate function, from which the phase birefringence as a function of wavelength is retrieved. We also determine the group birefringence dispersion. The functions measured in a range from 500 to 900 nm are compared with those resulting from the available dispersion relation, and very good agreement is confirmed.     

Roughness and fractality of fracture surfaces as indicators of mechanical quantities of porous solids

The 3D profile surface parameter H _q and fractal dimension D were tested as indicators of mechanical properties inferred from fracture surfaces of porous solids. High porous hydrated cement pastes were used as prototypes of porous materials. Both the profile parameter H _q and the fractal dimension D showed capability to assess compressive strength from the fracture surfaces of hydrated pastes. From a practical point of view the 3D profile parameter H _q seems to be more convenient as an indicator of mechanical properties, as its values suffer much less from statistical scatter than those of fractal dimensions.