Assessment of the retention properties of poly(vinyl alcohol) stationary phase for lipid class profiling in liquid chromatography

Potentialities of polymerized vinyl alcohol on silica gel were assessed for class separation of simple lipids, sphingolipids, glyceroglycolipids and phospholipids by high-performance liquid chromatography. A screening of pure solvents in binary gradient elution and a chemometric approach was used to define a rugged two segment linear gradient formed from four solvents for total lipid class separation. Triethylamine and formic acid were added in all mobile phase components for acidic phospholipid separation and evaporative light scattering response enhancement. Simple analytical procedures are described for the analysis of complex lipid materials.     

New Synthetic Approaches to Functionally Substituted 4,5-Dihydro-1,2,3-oxadiazole 2-Oxides

A practical procedure has been proposed for the synthesis of functionally substituted 4,5-dihydro-1,2,3-oxadiazole 2-oxides on the basis ofsulfamic acid derivatives.__________Translated from Zhurnal Organicheskoi Khimii, Vol. 41, No. 1, 2005, pp. 121–123.Original Russian Text Copyright © 2005 by Tartakovskii, Ermakov, Strelenko, Vinogradov, Petrov.     

Synthesis of N-substituted 2-benzoxalones

3-Acetylaminomethyl-2-benzoxazolones are obtained by Beckmann rearrangement of the anti-oximes of 3-acetonyl-2-benzoxazolones. The isomeric 3-(N-methylcarbamoylmethyl)-2-benzoxazolones are synthesized by alkylation of 2-benzoxazolone with chloroacetic acid, followed by reaction of the 3-carboxymethyl-2-benzoxazolones obtained with thionyl chloride and methylamine.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 9, pp. 1185–1188, September, 1985.     

Copolymers of the C9 hydrocarbon fraction of liquid pyrolysis products with maleic anhydride and their esterification products as additives to paper pulp

The influence exerted by copolymers of the C₉ fraction of liquid pyrolysis products of petroleum raw materials with maleic anhydride and by their esterification products, added to paper pulp, on the main paper properties was examined.     

MONOFUNCTIONAL3,4-and4',5'-PHOTOCYCLOADDUCTS BETWEEN 4,5'-DIMETHYLANGELICIN and THYMINE

By irradiating (365 nm) an aqueous liquid solution of 4,5'-dimethylangelicin. a monofunctional photosensitizing furocoumarin, in the presence of an excess of thymine, two new compounds, I and II, have been obtained; they do not show fluorescence when observed with Wood's light. The nuclear magnetic resonance data, the marked similarity of UV absorption and fluorescence spectra of these compounds with those of synthetic 3.4-dihydro-4,5'-dimethylangelicin and their capacity to undergo photodissociation (254 nm) yielding the starting thymine and 4,5'-dimethylangelicin in equimolecular amounts, are consistent with C₄-cycloadducts between the 3,4-double bond of the furocoumarin and 5,6-double bond of thymine. Nuclear magnetic resonance data indicate for I and II a head-to-head and a head-to-tail structure, respectively. When irradiation is carried out in the frozen state, two adducts. III and IV, fluorescent at Wood's light, have been obtained other than the two above-mentioned compounds I and II. Compounds III and IV have been identified as 4'.5'-fluorescent adducts between the 4',5'-double bond of the furocoumarin and the 5.6-double bond of thymine; one of them (III) is identical to that formed in the photoreaction between DNA and 4,5'-dimethylangelicin; for this last compound a cis head-to-head structure has been suggested.     

Temperature-programmed reduction and oxidation of bimetallic Pd?Ni/Al2O3 catalysts

Temperature-programmed reduction and oxidation of bimetallic catalysts Pd–Ni/Al₂O₃ seem to indicate phase segregation of palladium and nickel oxides and alloying of palladium and nickel in the process of reduction of oxidized catalysts.

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- Pd–Ni/Al₂O₃ , .

     

Tandem purification of mouse IgM monoclonal antibodies produced in vitro using anion-exchange and gel fast protein liquid chromatography

A tandem chromatographic procedure was used to isolate rapidly mouse IgM monoclonal antibodies produced by cultivation of hybridomas in vitro. Hybridoma culture supernatants containing mouse IgM monoclonal antibodies were first chromatographed on an anion-exchange Mono Q column connected to a fast protein liquid chromatography system. This anion-exchange step offers the advantage of obtaining IgM antibodies in a concentrated form. The IgM-rich fractions from the Mono Q column were then injected on a gel filtration Superose 6 column equilibrated with a low-ionic strength buffer and eluted with a high-ionic strength buffer. Assessment of the purity of isolated IgM monoclonal antibodies was performed by sodium dodecyl sulphate polyacrylamide gel electrophoresis together with a Coomassie Brillant Blue R 250 staining technique. Assessment of the immunoreactivity of isolated IgM monoclonal antibodies was performed by an enzyme linked immunosorbent assay using a solid phase adsorbed antigen against which IgM monoclonal antibodies were directed. The chromatographic procedures described allows the rapid isolation of mouse IgM monoclonal antibodies produced in vitro at a high degree of purity and in an immunoreactive state.     

Relations entre structure chimique et grandeurs de retention. VII. Composés de structure cyclopropanique

Résumé Les auteurs ont étudié le comportement chromatographique sur plusieurs phases stationnaires polaires et non polaires de composés cyclopropaniques stéréoisomêres: où R=H ou CH₃ et X=CH, COOCH₃ ou CH₂OH. Les résultats sont interprétés en fonction de la configuration de X par rapport à , de la nature électronique de X et de l'orientation du phényle par rapport au plan du cyclopropane.

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Relationship between chemical structure and retention. VII. Cyclopropane compounds

Summary The chromatographic behaviour, on several polar and non polar phases, of stereoisomeric cyclopropanes has been studied R=H or CH₃ and X=CN, COOCH₃, CH₂OH. The results are interpreted in terms of the X versus configuration, the electronic nature of X and the orientation of the phenyl ring in relation to plane of the cyclopropane ring.

     

A new method of removing excess of reagent from organic phases in the solvent extraction of metal complex anions with quaternary ammonium salts: Spectrophotometric determination of micro amounts of cobalt with 2-nitroso-1-naphthol-4-sulfonic acid

The removal of excess reagent extracted into an organic phase in the solvent extraction of a metal complex anion with a quaternary ammonium ion is discussed. With a given chelating ligand (HO—R—SO₃H), the order of extractability is HO—R—SO₃^- > M(OR—SO₃)^n- > X^- > ^-O—R—SO₃^- when an anion such as nitrate or halide is added. If suitable amounts of the anion are added, only the excess of reagent can be removed. The principle is applied to the extraction with zephiramine of the cobalt complex anion formed with 2-nitroso-1-naphthol-4-sulfonic acid. Micro amounts of cobalt in pure nickel salts were determined spectrophotometrically.     

Electrochemical detection of tryptophan metabolites following high-performance liquid chromatography.

Electrochemical detection of tryptophan metabolites following separation on a reversed-phase high-performance liquid chromatography column was compared with other means of detection. Of 29 compounds studied, 26 could be detected at a sensitivity comparable to that of fluorescence derivatisation procedures. Response was linear over a wide range of concentrations and selectivity was shown to be superior to ultraviolet detection when analysing urine. Additionally, it was possible to control selectivity so that only those tryptophan metabolites from the tryptophan hydroxylase pathway were detected. This is of particular value in the study of distrubances of serotonin metabolism and is unique to this type of detector.