Application of a rapid and selective method for the simultaneous determination of carebastine and pseudoephedrine in human plasma by liquid chromatography–electrospray mass spectrometry for bioequivalence study in Korean subjects

We describe a simple, rapid and sensitive high‐performance liquid chromatography–electrospray ionization tandem mass spectrometric method that was developed for the simultaneous determination of carebastine and pseudoephedrine in human plasma using cisapride as an internal standard. Acquisition was performed in multiple‐reaction monitoring mode by monitoring the transitions: m/z 500.43 > 167.09 for carebastine and m/z 166.04 > 147.88 for pseudoephedrine. The devised method involves a simple single‐step liquid–liquid extraction with ethyl acetate. Chromatographic separation was performed on a C₁₈ reversed‐phase chromatographic column at 0.2 mL/min by isocratic elution with 10 mM ammonium formate buffer–acetonitrile (30:70, v/v; adjusted to pH 3.3 with formic acid). The devised method was validated over 0.5–100 ng/mL of carebastine and 5–1000 ng/mL of pseudoephedrine with acceptable accuracy and precision, and was successfully applied to a bioequivalence study involving a single oral dose (10 mg of ebastine plus 120 mg of pseudoephedrine complex) to healthy Korean volunteers. Copyright © 2010 John Wiley & Sons, Ltd.     

Bentonite stability,speciation and migration behaviour of some critical radionuclides

The contribution is focused on chemical, geochemical and mineralogical research of bentonite stability with the aim to determine the effect of saturation medium composition and loading by heat on bentonite stability. The main part of the research is directed to the experimental results of bentonite and bentonite leachate samples obtained for the bentonite interaction under laboratory experiments. Computer-modeling methods were used to calculate equilibrium thermodynamic principles, the distributions of predominant aqueous species, and potential solubility controls for the environmentally important oxidation states of each investigated radioactive contaminants. The Eh–pH diagrams of individual chemical species of the tested radionuclides were calculated by the geochemical software tool Geochemist’s Workbench that included the actual chemical compositions of the solid–liquid systems under the given experimental conditions. It was confirmed that smectites are transformed to more stable silicate phases, such as illite/smectite mixed layers, illite. The data obtained from the model calculations conform with experimental results. The effect of the variable aqueous phase composition on bentonite stability using Ca–Mg and Na–Ca bentonites for the experiments was studied. The synthetic granitic waters with the higher concentration of the K⁺ and Mg²⁺ cations were applied for the study of bentonite stability.     

Acetylcholinesterase-Inhibiting Activity of Salicylanilide <em>N</em>-Alkylcarbamates and Their Molecular Docking

A series of twenty-five novel salicylanilide N-alkylcarbamates were investigated as potential acetylcholinesterase inhibitors. The compounds were tested for their ability to inhibit acetylcholinesterase (AChE) from electric eel (Electrophorus electricus L.). Experimental lipophilicity was determined, and the structure-activity relationships are discussed. The mode of binding in the active site of AChE was investigated by molecular docking. All the discussed compounds expressed significantly higher AChE inhibitory activity than rivastigmine and slightly lower than galanthamine. Disubstitution by chlorine in C'_(3,4) of the aniline ring and the optimal length of hexyl-undecyl alkyl chains in the carbamate moiety provided the most active AChE inhibitors. Monochlorination in C'₍₄₎ exhibited slightly more effective AChE inhibitors than in C'₍₃₎. Generally it can be stated that compounds with higher lipophilicity showed higher inhibition, and the activity of the compounds is strongly dependent on the length of the N-alkyl chain.     

Study of Interaction between Metallothionein and CdTe Quantum Dots

Quantum dots (QDs) belong to a new class of fluorescent agent for biochemical, medicinal or other purposes. However, QDs based on cadmium or other metals can be risky for an organism. As one of the mechanism how to detoxify cadmium-based QDs expression of metallothioneins (MT) can be considered. Due to high affinity of metallothionein to cadmium(II) ions, we attempted to develop an approach for studying of possible interaction with QDs. We prepared QDs with CdTe core and studied the interaction with MT, which we isolated from livers of Cd-administered rabbits. To study the interaction, we used the mixture of both components MT (3.6 μM): CdTe QDs (0, 0.34, 0.68, 1.02, 1.36, 1.7, 2.04 and 2.47 μM). The mixtures were studied by spectrophotometry within the range from 200 to 750 nm with detected maxima at 260 and 505 nm. Same mixtures were also analysed by differential pulse voltammetry Brdicka reaction, which supported data from spectrophotometry. Subsequently, we used fast protein liquid chromatography for purification of protein–quantum dot conjugates. We obtained the different chromatograms for (1) Apo MT, (2) CdTe QDs and (3) MT–QD complex. We also collected the fractions and subsequently analysed them on the content of Cd and MT, which confirmed the formation of CdTe QDs–MT complex.     

Mössbauer spectroscopy of goethite of small particle size

A series of synthetic acicular and natural goethite samples was examined by Mössbauer spectroscopy in the temperature range 5 to 290 K. From the temperature dependence of magnetic moment fluctuations the anisotropy constant has been estimated and the results have been compared with results of the magnetic measurements.     

An Application of a Multi-Objective Tabu Search Algorithm to a Bicriteria Flowshop Problem

This paper proposes a new tabu search algorithm for multi-objective combinatorial problems with the goal of obtaining a good approximation of the Pareto-optimal or efficient solutions. The algorithm works with several paths of solutions in parallel, each with its own tabu list, and the Pareto dominance concept is used to select solutions from the neighborhoods. In this way we obtain at each step a set of local nondominated points. The dispersion of points is achieved by a clustering procedure that groups together close points of this set and then selects the centroids of the clusters as search directions. A nice feature of this multi-objective algorithm is that it introduces only one additional parameter, namely, the number of paths. The algorithm is applied to the permutation flowshop scheduling problem in order to minimize the criteria of makespan and maximum tardiness. For instances involving two machines, the performance of the algorithm is tested against a Branch-and-Bound algorithm proposed in the literature, and for more than two machines it is compared with that of a tabu search algorithm and a genetic local search algorithm, both from the literature. Computational results show that the heuristic yields a better approximation than these algorithms.     

Characterization and kinetic study of sunflower oil and biodiesel

In this study, the physico-chemistry characterization and kinetic study of the thermal decomposition of sunflower oil and its biodiesel were carried out. Sunflower biodiesel was synthesized by the methanol route and basic homogeneous catalysis. The physicochemical characterization of the sunflower oil and biodiesel were performed according to standards set out in the ANP resolution, and both are in accordance to the specifications. The chromatographic analysis was obtained by GC-FID. The yield of conversion of 97.4 wt% of sunflower oil in methyl esters confirms the efficiency of the conversion of the fatty acids into esters. The thermal analysis was performed on a thermobalance, using heating rates of 5, 10, and 20 °C min⁻¹. In these three rates, we observed a single well-defined step of mass loss that describes the volatilization and decomposition of the sunflower oil and the biodiesel. The kinetic study was performed using equations of approximation and integration methods such as Coats–Redfern, Van Krevelen, and Horowitz–Metzger. The kinetic parameters reaction order (n) and apparent activation energy (E _a), obtained by applying these method were correlated.     

A comparison of classical 90Sr separation methods with selective separation using molecular recognition technology products AnaLig? SR-01 gel, 3M Empore? Strontium Rad Disk and extraction chromatography Sr?Resin

We studied the use of an extraction chromatography for determination of ⁹⁰Sr in contaminated water samples. The aim of our work was to compare selected products from the point of view of the strontium chemical yields and analysis time. Three commercial products, 3M Empore? Strontium Rad Disk, AnaLig^® Sr-01 gel, Sr^®Resin, and two classical methods, liquid?Cliquid extraction with tributhylphosphate and carbonate co-precipitation, were tested for the separation of ⁹⁰Sr. The water sample from nuclear power plant A1 Jaslovske Bohunice was used for radiochemical analysis of ⁹⁰Sr volume activity. Samples were traced with ⁸⁵Sr to monitor strontium chemical recovery and counted either by Cerenkov counting on TRI CARB 2900 TR liquid scintillation counter or low level alpha?Cbeta proportional counter.