Méthode de marquage de groupes carboxyliques dans les peptides. Propriétés chromatographiques et autres,de peptide-p,p′-dimapa-anilides

Résumé Les auteurs décrivent une méthode efficate et les conditions (faibles valeurs de pH, milieu dioxane/eau (1∶2), carbodiimide hydrosoluble) de formation de peptides colorés par réaction de leur groupe carboxylique avec un colorant aminé (par exemple: 1(4-diméthylamino-1 phénylazo)-4-aminobenzène=p,p′-dimapa-aniline), sans polymérisation du peptide non-protégé. Quelques méthodes chromatographiques, faciles à mettre en oeuvre, pour l'isolement de peptide-p,p′-dimapa-anilides et quelques propriétés de ces nouveaux composés (peptides-C-colorés) sont présentées.

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Method for labelling carboxylic groups in peptides. Chromatographic and other properties of peptide-p,p′-dimapa-anilides

Summary The authors describe an effective method and the conditions (low pH values, dioxane/water (1∶2) media, watersoluble carbodiimide) for making coloured carboxylic peptides from amino-dye (i.e.: 1(4-dimethylamino-1 phenylazo)-4-aminobenzene=p,p′-dimapa-aniline), without polymerisation of unprotected peptide. Some easy chromatographic methods for isolation of peptide-p,p′-dimapa-anilides and some properties of these new compounds (C-dyed-peptides) are given.

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Reaction of ethyl perfluoromethacrylate with [η5-C5H5Fe(CO)2]− anion

Conclusions The cis-trans isomers of the vinylic fluorine substitution product were isolated and characterized when Na[⁵-C₅H₅Fe(CO)₂] is reacted with ethyl perfluoromethacrylate.Deceased.The authors express their gratitude to E. M. Rokhlin and U. Utebaev for supplying the ethyl perfluoromethacrylate.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 3, pp. 705–706, March, 1977.     

Assay of flurazepam in plasma by differential pulse polarography

Analytical and Bioanalytical Chemistry - A combination of differential solvent extraction based on physical chemical properties of the species involved and differential pulse polarography has been...     

Gas chromatographic determination of estrone,estradiol and estriol in non-pregnancy plasma

Summary A gas Chromatographic method for the determination of estrone, estradiol and estriol in plasma of normal females is described. Purification is done by means of TLC of the free compounds and the acetates and quantitation is achieved by electron capture-gas chromatography of the estrogen heptafluorobutyrates. Experiments on the validation of the method are described along with some examples of its application.

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Zusammenfassung Eine gaschromatographische Methode zur Bestimmung von Östron, Östradiol und Östriol im normalen weiblichen Plasma wurde beschrieben. Die Reinigung erfolgte durch Dünnschichtchromatographie der freien Verbindungen und ihrer Acetate. Die quantitative Bestimmung wurde gaschromatographisch mit Hilfe eines Elektroneneinfangdetektors an Hand der Östrogenheptafluorobutyrate bewerkstelligt. Versuche zur Bewertung dieser Methode sowie Beispiele für ihre Anwendung wurden beschrieben.

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Supported by USPHS Grants AM 09908 and RCDA 5 K 3-AM-31, 321 (S. K.) and a grant from the Ford Foundation.     

Acetals of lactams and acid amides. 35. Synthesis of condensed two- and three-ring pyridine systems on the basis of enamino amides

The synthesis of 2,3,5,6-tetrahydropyrrolo[3,2-c]pyrid-6-one was accomplished by rearrangement of 8H,1-cyano-8-dimethylaminomethylene-2,5,6,7-tetrahydropyrrolo[1, 2-c]pyrimidine. Pyrrolo[3,2-c]pyrimidine, 1,6-naphthyridine, and pyrimido[4,3-b]-azepine derivatives were synthesized on the basis of enamino dinitriles. The hydrolysis of 8H,1-cyano-8-dimethylaminomethylene-2,5,6,7-tetrahydropyrrolo[1,2-c]-pyrimidine in 50% CH₃COOH leads to a pyrrolo[1,2-c]pyrido[4,3-d]pyrimidine derivative. A similar dipyrido[4,3-d-1,2-c]pyrimidine derivative was obtained from 1-cyano-9-dimethylaminomethylene-2,5,6,7,8,9-hexahydropyrido[1,2-c]pyrimidine under these conditions, and 3,4-dioxo-3,4,7,8,9,10-hexahydropyrido[1,2-c]pyrano[4,3-d]-pyrimidine was synthesized bytreatment with a 1 N solution of HCl.See [1] for Communication 34.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 4, pp. 518–522, April, 1982.     

Analysis and parametric sensitivity of the behavior of overshoots in the concentration of a charged adsorbate in the adsorbed phase of charged adsorbent particles: practical implications for separations of charged solutes

In this work, an analysis of the parametric sensitivity of the overshoot in the concentration of the adsorbate in the adsorbed phase, which occurs under certain conditions during an ion-exchange adsorption process, is presented and used to suggest practical implications of the concentration overshoot phenomenon on operational policies and configurations of chromatographic columns and finite bath adsorption systems. The results presented in this work demonstrate and explain how the development of an overshoot in the concentration of the adsorbate in the adsorbed phase could be enhanced or suppressed by (i) varying the diffusion coefficient, D3, of the adsorbate relative to the diffusion coefficients, D1 and D2, of the cations and anions, respectively, of the background/buffer electrolyte, (ii) altering the initial surface charge density, delta0, of the charged adsorbent particles, (iii) varying the Debye length, lambda, and (iv) changing the initial concentration, Cd3(0), of the adsorbate in the bulk liquid of the finite bath. The influence of the pH and ionic strength, Iinfinity, of the liquid solution on the development of an overshoot in the concentration of the adsorbate in the adsorbed phase is also presented and discussed through the relationships of these parameters to delta0 and lambda, respectively. Furthermore, a detailed explanation of the effects of each parameter on the interplay between the diffusive and electrophoretic molar fluxes, as well as on the structure and functioning of the electrical double layer, which are responsible for the concentration overshoot phenomenon, is presented.