Use of galvanostatic coulometry in the analysis of arbidol drug

Arbidol is proved to easily and completely react with electrogenerated bromine in the ratio 2: 9; so procedures for the arbidol quantification in the neat substance and drugs are developed, the RSD value does not exceed 2%. A procedure for the coulometric determination of water in the arbidol substance using the Fisher method is proposed.     

Optimization and validation of organochlorine compounds in adipose tissue by SPE‐gas chromatography

Scientific evidence has shown an association between organochlorine compounds (OCC) exposure and human health hazards. Concerning this, OCC detection in human adipose samples has to be considered a public health priority. This study evaluated the efficacy of various solid‐phase extraction (SPE) and cleanup methods for OCC determination in human adipose tissue. Octadecylsilyl endcapped (C₁₈‐E), benzenesulfonic acid modified silica cation exchanger (SA), poly(styrene‐divinylbenzene (EN) and EN/RP₁₈ SPE sorbents were evaluated. The relative sample cleanup provided by these SPE columns was evaluated using gas chromatography with electron capture detection (GC–ECD). The C₁₈‐E columns with strong homogenization were found to provide the most effective cleanup, removing the greatest amount of interfering substance, and simultaneously ensuring good analyte recoveries higher than 70%. Recoveries > 70% with standard deviations (SD) < 15% were obtained for all compounds under the selected conditions. Method detection limits were in the 0.003–0.009 mg/kg range. The positive samples were confirmed by gas chromatography coupled with tandem mass spectrometry (GC‐MS/MS). The highest percentage found of the OCC in real samples corresponded to HCB, o,p′‐DDT and methoxychlor, which were detected in 80 and 95% of samples analyzed respectively. Copyright © 2012 John Wiley & Sons, Ltd.     

1H NMR Study on the Isomerization of 2,4,6-Triphenyl-4H-Seleno(Thio)Pyrans

It is shown using ¹H NMR spectroscopy that 2,4,6-triphenyl-4H-seleno(thio)pyrans can be isomerized into 2H-isomers by the action of lithium perchlorate or lithium chloride in DMF or only by DMF. The reaction time is found to depend on the Lewis acidity of used salt. It is supposed that isomerization in presence of Lewis acids proceeds as endocyclic 1,3-proton transfer or as a series of two 1,2-hydride shifts.     

Olefin Synthesis via,the Li-Derivative of N,N,N′,N′-Tetramethyldimides of Arylmethanephosphonic Acids

Abstract

The high erythro-stereoselective reaction of Li-tetramethyldiamides of arylmethanephosphonic acids with carbonyl compounds is used for synthesis of (Z)-alkenes by thermolysis of the erythro-adducts as well as in acidic media.     

Investigation of the molecular mobility of peptin macromolecules using photon-correlation spectroscopy

The pH dependence of the intermolecular interaction coefficient of pepsin in an aqueous solution is obtained by using photon-correlation spectroscopy. The dependence shows a minimum near the isoelectric point (pH 1.6). The dynamic parameters of pepsin macromolecules in solutions containing various metal ions, including potassium, cobalt, lead, cesium, and rubidium are studied. It is shown that the addition of these ions causes a decrease of the translational diffusion coefficients. It is found that an increase in temperature leads to the structural transition of a pure solution of pepsin in water. The activation energy of this transition is calculated using the Arrhenius law.     

Mechanical properties and energy dissipation in ultrafine-grained AMts and V95 aluminum alloys during dynamic compression

The thermomechanical characteristics of ultrafine-grained AMts and V95 aluminum alloys with an average crystallite size of 200–600 nm are experimentally studied during dynamic compression. The alloys are fabricated by dynamic channel angular pressing. It is found that the deformation history of the alloys and the initial characteristics of their structural state affect the subsequent plastic deformation and the dissipation of applied energy. The studies of the thermodynamics of deformation in combination with structural investigations before and after dynamic compression allowed us to reveal the main structural relaxation mechanisms in the materials during dynamic compression and to determine the dissipation abilities of various defect structures.     

STEREOSELECTIVITY OF THE WITTIG-HORNER REACTION WITH BENZYLPHOSPHONATE CARBANIONS AND ALDEHYDES

Abstract

The interaction of Li-diethylbenzylphosphonate 1-Li with aldehydes 2 is studied at different reaction conditions, the corresponding β-hydroxyethanephosphonate 3 being isolated. It is found that in these cases the aldol stage of the HWE reaction is not stereoselective or threo isomers predominate. The elimination stage leads only to trans-alkene due to the electron and steric influence of the substituents at the phosphorus atom.