The alicyclic ring contraction of perfluoro-1-phenyltetralin in reaction with antimony pentafluoride

Perfluoro-1-phenyltetralin (1) heated with antimony pentafluoride at 130 °C, then treated with water, gave a mixture of perfluorinated 3-methyl-2-phenylindenone (3), 3-methyl-2-phenylindene (4), 3-hydroxy-1-methyl-3-phenylindan (5), 1-methyl-3-phenylindan (6), 9-methyl-1,2,3,4,5,6,7,8-octahydroanthracene (7), and 1,9-dimethyl-5,6,7,8-tetrahydro-β-naphthindan (8). When heated with SbF₅ in the presence of HF, then treated with water, compound 1 is transformed to a mixture of products 3-6. The reaction at 170 and 200 °C forms compounds 3-6 together with perfluoro-2-(cyclohexen-1-yl)-3-methylindene (10).     

Generation of peptide radical dications via low-energy collision-induced dissociation of [Cu<Superscript>II</Superscript>(terpy)(M + H)]<Superscript>·3+</Superscript>

The first example of the formation of hydrogen-deficient radical cations of the type [M + H](.2+) is demonstrated to occur through a one-electron-transfer mechanism upon low-energy collision-induced dissociation (CID) of gas-phase triply charged [Cu(II)(terpy)(M + H)](.3+) complex ions (where M is an angiotensin III or enkephalin derivative; terpy = 2,2':6',2'-terpyridine). The collision-induced dissociation of doubly charged [M + H](.2+) radical cations generates similar product ions to those prepared through hot electron capture dissociation (HECD). Isomeric isoleucine and leucine residues were distinguished by observing the mass differences between [z(n) + H](.+) and w(n)(+) ions (having the same residue number, n) of the Xle residues. The product ion spectrum of [z(n) + H](.+) reveals that the w(n)(+) ions are formed possibly from consecutive fragmentations of [z(n) + H](.+) ions. Although only the first few [M + H](.2+) species have been observed using this approach, these hydrogen-deficient radical cations produce fragment ions that have more structure-informative patterns and are very different from those formed during the low-energy tandem mass spectrometry of protonated peptides.     

Corrected results for the influence of size,zeta potential,and state of motion of dispersed particles on the conductivity of a colloidal suspension

A correction of a recent work on the dependence of the DC conductivity of diluted colloidal suspensions on the size, zeta potential, and state of motion of dispersed particles (C. Grosse, S. Pedrosa, V.N. Shilov, J. Colloid Interface Sci. 251 (2002) 304) is presented. It is shown that the procedure used in that work to calculate the contribution of the particles to the conductivity of the suspension leads to a result that includes the variation of the conductivity of the dispersion medium. Revised analytical and numerical calculations are presented, which strongly reinforce the conclusions reached in the original work: The expression for the conductivity increment based on the value of the dipolar coefficient of the suspended particles (calculated taking into account their electrophoretic motion) appears to be valid over the whole range of particle sizes.     

Exploring bioanalytical applications of assisted protein reassembly

Reassembly of protein from its peptide fragments is a technique that can have many applications in the bioanalytical field. Typically, a reporter protein fragmented into its two peptides is employed as a label in this study. This fragments of peptide can reassemble yielding an active functional reporter. This reassembly of the protein can be assisted by non-covalently interacting peptides or proteins, which are attached to the fragmented reporter. This technique has been employed in several applications including study of protein–protein interactions, antibody screening, immunoassays, and high-throughput screening. This review focuses on different reporters employed in the study of reassembly of proteins and applications of this strategy in bioanalysis.     

Transport in ceria electrolytes modified with sintering aids: effects on oxygen reduction kinetics

Small (2 mol%) cobalt oxide additions to ceria-gadolinia (CGO) materials considerably improve sinterability, making it possible to obtain ceramics with 95–99% density and sub-micrometre grain sizes at 1,170–1,370 K. The addition of Co causes a significant shift of the electrolytic domain to lower pO₂. This modification to the minor electronic conductivity of the electrolyte material has influence on the cathodic oxygen reduction reaction. The impedance technique is shown to provide information not only about polarisation resistance, but also about the active electrode area from analysis of the current constriction resistance. It is demonstrated that this current constriction resistance can be related to the minor electronic contributions to total conductivity in these materials. A simple imbedded grid approach gives control of the contact area allowing the properties of the electrolyte materials to be studied. A much lower polarisation resistance for the Co-containing CGO electrolyte is observed, which can be clearly attributed to an increased three-phase reaction area in the Co-containing material, as a consequence of elevated p-type conductivity.     

Application of high-performance liquid chromatography of some antibiotics in clinical microbiology

During recent years high-performance liquid chromatography has become an excellent tool for the determination of antibiotics in biological fluids. Compared with biological assays, the major benefits of this method are specificity and rapidity. In particular, the determination of biologically inactive metabolites emphasizes that this technique plays an outstanding role for the analysis of antibiotics. This paper describes how the method can be used in the analysis of several antibiotics and demonstrates the efficacy of this method for clinical microbiology. Methods for the determination in biological fluids of acylaminopenicillins (azlocillin, mezlocillin, piperacillin and aspoxicillin), quinolones (ciprofloxacine, norfloxacine and ofloxacine), a penem (imipenem) and a cephalosporin (cefixime) are summarized. Furthermore, their application to in vitro studies and their trial in clinical studies are described.     

Preparation of Fe/B powders by mechanical alloying

Steels with a high boron content are valuable as a neutron shield in waste containers and as control absorbers in nuclear reactors. The purpose of this study was to obtain by mechanical alloying an iron powder with 50% boron (by weight) and then powder-metallurgy materials. The elementary powders were mixed in a high-energy mill for 36 h in an inert atmosphere. Samples were withdrawn at intervals, and the powder was characterized by differential thermal analysis, X-ray diffraction and electron microscopy. The Fe/B powders withdrawn at different intervals of milling were diluted with further additions of iron up to a final content of 10% boron. The mixtures were uniaxially compacted at 500 MPa; their green density was verified, and they were sintered in argon at 1150°C. Their physical properties (density and dimensional change) and bending strength were evaluated and microstructural studies and fracture tests were performed.     

Electrocatalytic properties of surface oxides on gold,platinum, and stainless steel electrodes in electrooxidation of malic acid

Electrocatalytic properties of oxides formed at gold, platinum, and stainless steel electrodes in the malic acid electrooxidation in 0.1 M Na₂SO₄ are studied. Gas chromatographic analysis of the electrolyte after holding the potential at 1.0 V for 8 h shows that on platinum and gold electrodes 2 mmol of acetaldehyde are produced and on stainless steel, 45 mmol. The acetaldehyde yield is the highest on stainless steel.From Elektrokhimiya, Vol. 41, No. 3, 2005, pp. 304–309.Original English Text Copyright © 2005 by Avramov Ivi, Popi, Antonovi.This article was submitted by the authors in English.     

Preparation of weak cation exchange packings based on monodisperse poly(glycidyl methacrylate-<Emphasis Type="Italic">co</Emphasis>-ethylene dimethacrylate) beads and their chromatographic properties

The monodisperse, macroporous poly(glycidyl methacrylate- co-ethylene dimethacrylate) beads were synthesized by a single-step swelling and polymerization method. Based on this media, a weak cation exchange (WCX) stationary phase for HPLC was synthesized by a new chemically modified method. The prepared resin has advantages for biopolymer separation, high column efficiency, low column backpressure, high protein mass recovery, and good resolution for proteins. The measured bioactivity recovery for lysozyme was 98+/-5%. The dynamic protein loading capacity of the WCX packings was 17.3 mg g(-1). The experimental results show that the synthesized WCX resin has very weak hydrophobicity.     

Analysis of steroids. XLI. Ion-pair high-performance liquid chromatographic separation of quaternary ammonium steroids on silica.

A normal-phase ion-pair chromatographic system has been developed for the high-performance liquid chromatographic investigation of pipecuronium bromide (2 beta,16 beta-bis-(N'-dimethyl-l-piperazinyl)-3 alpha,17 beta-diacetoxy-5 alpha-androstane dibromide) and related quaternary ammonium steroids. The use of silica as the stationary phase and a 96:4 mixture of acetonitrile and water containing 0.1 mol/dm3 sodium perchlorate as the eluent with detection at 213 nm enable the potential impurities as well as the hydrolytic and oxidative degradation products of pipecuronium bromide to be separated and detected down to the 0.01% level. The above system is also applicable to the high-performance liquid chromatographic investigation of other quaternary ammonium steroids (pancuronium bromide, vecuronium bromide).