Reversed-phase high performance liquid chromatographic method for the determination of lansoprazole, omeprazole and pantoprazole sodium sesquihydrate in presence of their Acid-induced degradation products

A simple sensitive, selective and accurate reversed-phase high performance liquid chromatographic method was developed and validated for the quantitative determination of lansoprazole, omeprazole and pantoprazole sodium sesquishydrate in the presence of their acid-induced degradation products. The three compounds were monitored at 280 nm using Nova-Pak C(18) column and a mobile phase consisting of 0.05 M potassium dihydrogen phosphate : methanol : acetonitrile (5 : 3 : 2 v/v/v). Linearity ranges were 2-20 mug ml(-1), 2-36 mug ml(-1) and 0.5-20 mug ml(-1) for lansoprazole, omeprazole and pantoprazole, respectively. The corresponding recoveries were 100.61+/-0.84%, 100.50+/-0.80% and 99.78+/-0.88%. The minimum detection limits were 0.55, 0.54 and 0.03 mug ml(-1) for lansoprazole, omeprazole and pantoprazole, respectively. The method could be successfully applied to the determination of pure, laboratory prepared mixtures and pharmaceutical dosage forms. The results obtained were compared with the reported methods for lansoprazole and pantoprazole or the official U.S.P method for omeprazole.     

Synthesis and characterization of silver(I) coordination networks bearing flexible thioethers: anion versus ligand dominated structures

This report describes the synthesis and X-ray characterization of a series of L(n)AgX complexes wherein Ln = PhS(CH2)nSPh (n = 2, 4, 6, 10) and X = CF3SO3-, CF3COO-, CF3CF2COO-, CF3CF2CF2COO-, NO3-, and ClO4-. This study was undertaken in order to rationalize the structure of the coordination networks formed as a function of the anion coordinating strength and the ligand structure. The following complexes were examined: with L(2), CF3SO3- (1), CF3COO- (2), ClO4- (3); L4, CF3SO3- (4), CF3COO- (5), CF3CF2COO- (6), CF3CF2CF2COO- (7); L6, CF3COO-.H2O (8), CF3CF2COO- (9), CF3CF2CF2COO- (10); and L10, NO3- (11). The anions selected are classified in three groups of increasing coordinating strength: perchlorates, fluorosulfonates, and perfluorocarboxylates. Except in two cases, all complexes form 2D-coordination networks. The 2D-network in 1 (L2, CF3SO3-) is made up of Ag(I) and L2, while the anion is only a terminal co-ligand that completes the trigonal coordination around Ag(I). In 4 (L4, CF3SO3-), a 1D-coordination polymer, [Ag-L4-]infinity, is observed where the anions are coordinated to Ag(I) in a trigonal fashion. The perfluorocarboxylates form tetrameric units in a zigzag shape, but only with the L4 ligand. In these (6 and 7), the silver-silver distances are very short, especially those of the central bond, indicating the presence of weak Ag-Ag interactions. Dimers, with short silver-silver distances, are observed with ligands L2 and L6 and perfluorocarboxylates. In 8 (L6, CF3COO-.H2O), a 3D channel-like structure is built through water molecules that connect adjacent layers. An unusual stoichiometry is noted in 3 (L2, ClO4-, acetone); Ag:L is 4:2.5. In 11 (L10 and NO3-), the nitrate acts as a bidentate ligand and an [Ag-NO3-]infinity chain is formed. Adjacent chains are linked by the L10 ligands into a 2D-coordination network.     

15N allocation into wheat grains (Triticum aestivum L.) influenced by sowing rate and water supply at flowering under a Mediterranean climate

This study examined the effects of a reduced wheat sowing rate (250 vs. 500 grains m^–2) on grain yield, uptake of ¹⁵N into grains, and the incorporation into gluten and non-gluten proteins of wheat under field conditions in the Aegean region. A single ¹⁵N application was applied at stem elongation, at flowering, or at both developmental stages. Each ¹⁵N treatment included either additional water supply, or no additional water supply at flowering. Sowing rate (either 250 or 500 grains m^–2) had no impact on grain yield. Grain yield increased with additional water supply, but at the expense of protein quality, because of a decrease in the protein content of gluten. The ¹⁵N content of the gluten and non-gluten proteins at grain maturity was not different among cultivars. ¹⁵N applied at both stem elongation and flowering was found in comparable amounts in grains and protein fractions, irrespective of sowing rate.     

A phenomenological model for the simulation of functional fatigue in shape memory alloy wires

In this contribution, a modelling framework for functional fatigue in shape memory alloy wires is introduced. The approach is in particular designed to reproduce the effective response determined by experiments as published in, e.g., Eggeler et al. (Mat Sci Eng A 378:24–33, 2004). In this context, the decrease of transformation stresses, the increase of irreversible strains, and the occurrence of “characteristic points” with respect to the stress-strain relation is explicitly covered in the model formulation. The modelling approach for the phase transformations itself offers a large potential for further micromechanically well-motivated model extensions.     

Computational models for proton transfer in biological systems

A computational scheme based on a “mixed basis set” approach is applied to the study of the structure and the energetics in proton transfer systems. Five hydrogen-bonded systems of the type (CH₃H_nA ‥ H ‥ BH_mCH₃)⁺, where A and B can be N, O, or S, have been investigated with various minimal and extended basis sets. Calculations with the extended basis set yield double-well potential energy curves, which the minimal basis set is unable to reproduce. Calculations with the mixed basis set, constructed from an extended basis set on the atoms engaged in the hydrogen transfer part and a minimal basis set on the rest of the molecule, give predictions of geometries, potential energy curves, and relative energies similar to the results from the extended basis set. Inclusion of polarization functions in the mixed basis set becomes essential in systems that contain third row atoms. This scheme should become useful in studies of large molecules in which different parts can be represented at different levels of computational complexity.     

Linear programming based meta-heuristics for the weighted maximal planar graph

The weighted maximal planar graph (WMPG) is practically important in the laying out of facilities in modern manufacturing environments. Given a weighted complete graph, the WMPG seeks to find a sub-graph such that it is planar—it can be embedded on the plane without any arcs intersecting, and it is maximal—no additional arc can be added to the sub-graph without destroying its planarity, and it also has the maximal sum of arc weights. In this paper, an integer linear programming (ILP) model is newly introduced for the problem. Two meta-heuristics are then derived from the ILP relaxation. The first meta-heuristic considers all variables with fractional values greater than half in the ILP relaxation to build an initial sub-graph from which a planar sub-graph is extracted using greedy random adaptive search procedure (GRASP) and augmented by triangulation of faces. The second meta-heuristic considers only arcs with integer values in the ILP relaxation. The remaining arcs are then sorted in descending order of their weights, for selection and insertion with a planarity testing procedure, to obtain a feasible solution using GRASP. Computational results are reported on a set of 100 test instances of size varying from 20 to 100 facilities. The computational results demonstrate the tightness of the new upper bound when compared to the classical one as well as the good performance of the proposed metaheuristics when compared to the best-known procedures in the literature in terms of solution quality and computational requirement. Finally, the paper presents a successful integration of GRASP with classical optimisation approaches and should be attempted for other optimisation problems.     

Broad Nematic Phases with High Clearing Points

Unbranched 4-(4′-alkylbenzoyloxy)-, 4-(4′-methylanlinobenzoyloxy)- and 4-(4′dime thylaminobenzoyloxy)benzylidene-4″-cyanoanmlines were synthesized. They show broad nematic phases with high nematic isotropic transitions. Lateral Clsubstituents decrease the clearing points of these liquid crystals by about 80°. The intermediate 4-(4′-alkylbenzoyloxy)benzaldehydes are monotropic nematic.     

Photoredox laser chemistry of transition metal oxides

Received: 26 May 1997/Accepted: 17 July 1997     

Eriochrome black A as reagent for spectrophotometric microdetermination of cobalt in presence of nickel

Summary Eriochrome black A has been found to be a suitable reagent for the spectrophotometric determination of microgram quantities of cobalt in pure cobalt solutions and in the presence of nickel and some other cations by measuring the decrease in the absorbance of Eriochrome black A at p_H 10, caused by the presence of cobalt.Many foreign cations especially nickel were completely masked by EDTA. Amounts as low as about 0.9 to 3 g were determined with fair accuracy.