Improvement of the chromatographic separation of several 1,4-dihydropyridines calcium channel antagonist drugs by experimental design

A high-performance liquid chromatographic method with diode array detection has been developed and optimized for the separation of five calcium channel blockers belonging to the 1,4-dihydropyridine subgroup (nifedipine and related drugs). The possibility of the simultaneous drug analysis allows a decrease of time during the assay as well as a saving of reagents and solvents. In this work, the effect of four experimental parameters (organic modifier percentage, pH value, concentration of the buffer in the mobile phase, and column temperature) on the chromatographic resolution are investigated by experimental design in order to optimize the chromatographic separation of five 1,4-dihydropyridines (amlodipine, nitrendipine, felodipine, lacidipine, and lercanidipine). Fractional factorial design, central composite design, and finally the Multisimplex program are used to establish the optimal conditions in terms of resolution and minimum analysis time. Optimal separation of the five compounds under study is achieved in less than 12 min using a Sulpecosil LC-ABZ+Plus C18 column, a composition of mobile phase of acetonitrile-10mM acetic acid acetate buffer pH 5 (72:28, v/v) at a flow rate of 1 mL/min, a column temperature of 30 degrees C +/- 0.1 degrees C, and a detection wavelength of 238 nm.     

Hydrophobic interaction effects on the kinetics of ligand substitution in binary aqueous mixtures at pentacyano(piperidine)ferrate(II) ion

The kinetics of piperidine replacement by pyridine at the pentacyano(piperidine)-ferrate(II) complex ion was studied under pseudo-first order conditions in binary aqueous mixtures of methanol, t-butanol, p-dioxane, and glycerol, from a mole fraction of co-solvent from 0 to about 0.15. The observed variations can be explained considering the degree of hydrophobic interaction between released ligand and water molecules which changes according to the structure-forming or struucture-breaking effect of added co-solvent on water.     

Epitaxial superconducting δ-MoN films grown by a chemical solution method

The synthesis of pure δ-MoN with desired superconducting properties usually requires extreme conditions, such as high temperature and high pressure, which hinders its fundamental studies and applications. Herein, by using a chemical solution method, epitaxial δ-MoN thin films have been grown on c-cut Al(2)O(3) substrates at a temperature lower than 900 °C and an ambient pressure. The films are phase pure and show a T(c) of 13.0 K with a sharp transition. In addition, the films show a high critical field and excellent current carrying capabilities, which further prove the superior quality of these chemically prepared epitaxial thin films.     

Formation and crystal structure of an exocyclic enol δ-lactone obtained from dimedone and trimethylsilylethynyl phenyliodonium triflate

The reaction between dimedone anion and trimethylsilylethynyl phenyliodonium triflate leads to the formation of 4,4-dimethyl-6-(1,5-bistrimethylsilylpentane-1,4-diyne-3-ylidene)-δ-valerolactone, whose crystal structure has been determined.     

Thermogravimetric analysis of polyester/cotton blends treated with Thpc-urea-poly(vinyl bromide)

Polyester/cotton fabric swith blend ratios of 0/100, 11/89, 20/80, 30/70, 50/50, and 65/35 were investigated via thermogravimetric analysis in both nitrogen and air atmospheres. The samples were heated from ambient to 750°C at a heating rate of 5°C min^?1. The same fabrics were analyzed after treatment with tetrakis (hydroxymethyl) phosphonium chloride-urea-poly(vinyl bromide) (Thpc-urea-PVBr) flame retardant.Weight losses observed during pyrolysis were assigned to the cotton and polyester portions of the blends. Both cotton and polyester thermally decompose to yield gases and solid char byproducts. In nitrogen the 100% cotton fabric undergoes one major weight loss between 270 and 370°C, with the maximum rate of weight loss, 0.15 mg/min-mg occurring at 346°C. Thermal decomposition of the 100% polyester occurs over a range of 335–470°C, with the peak rate of weight loss, 0.11 mg/min-mg, measured at 416°C. In an air atmosphere, both volatile gases and solid char by- products of pyrolysis undergo combustion. The combustion reactions are associated with measured weight losses. The maximum rate of weight loss for the cotton portion increases to 0.25 mg/min-mg and occurs at 317°C. The maximum rate of polyester decomposition remains the same in both air and nitrogen, but the temperature decreases to 405°C.     

Synthesis and mass spectra of some 1-aroylamino-5-arylaminomethyl-1,2,3-triazoles

The title compounds 2 are prepared from the reaction of 1-(N, N-diaroyl)amino-5-bromomethyl-1,2,3-triazoles with aromatic amines. The fragmentation pattern upon electron impact at 70 eV of compounds 2 is studied. The molecular ion peak is present in all the spectra examined. Besides the [M-28]⁺⁺, there is also a more abundant [M-29]⁺ peak, corresponding to a N₂H loss of the molecular ion. The ion Ar²NH = CH₂ is the base or the most prominent peak.     

Pointwise Estimates and Regularity in Geometric Optics and Other Generated Jacobian Equations

The study of reflector surfaces in geometric optics necessitates the analysis of certain nonlinear equations of Monge‐Ampère type known as generated Jacobian equations. This class of equations, whose general existence theory has been recently developed by Trudinger, goes beyond the framework of optimal transport. We obtain pointwise estimates for weak solutions of such equations under minimal structural and regularity assumptions, covering situations analogous to those of costs satisfying the A3‐weak condition introduced by Ma, Trudinger, and Wang in optimal transport. These estimates are used to develop a C^1,α regularity theory for weak solutions of Aleksandrov type. The results are new even for all known near‐field reflector/refractor models, including the point source and parallel beam reflectors, and are applicable to problems in other areas of geometry, such as the generalized Minkowski problem.© 2017 Wiley Periodicals, Inc.     

Resolution and identification of co‐eluting alkylphenols in comprehensive two‐dimensional gas chromatography–mass spectrometry by multivariate curve resolution‐alternating least squares

The interest in the analysis of alkylphenols (APs) has widely increased in the last decades because of the endocrine disrupting features of these phenol derivatives. However, the isolation and identification of many of the multiple chemical structures of all APs is a very challenging task because of their similar physicochemical properties. In this work, the co‐elution of the isomers present in technical mixtures and using comprehensive two‐dimensional gas chromatography coupled to quadrupole mass spectrometry was resolved using multivariate curve resolution‐alternating least squares algorithm. The mass spectrum of each resolved compound was compared with the theoretical mass spectrum obtained from the literature, in order to assign the appropriate identification of each isomer. Two commercial mixtures were studied; in one of them, 34 compounds were resolved, and in the second mixture, 40 compounds were resolved. The relative abundances of the compounds were also calculated in both mixtures. Copyright © 2015 John Wiley & Sons, Ltd.