Multi-analyte HPLC–DAD Method for Concurrent Analysis of Six Antimicrobials and Three Proton Pump Inhibitors Frequently used in Management of Helicobacter pylori Infection: Application to Simulated Intestinal Fluid Samples

Chromatographia - The present work deals with the optimization, validation and application of a versatile HPLC–DAD method for concurrent estimation of nine antimicrobials and proton pump...     

A recent approach for the synthesis of 1,2,4-triazine systems bearing and/or containing phosphorus atoms as donor-acceptor interaction and their biocidal affects: An overview

Abstract

This review reports the developed methods for the synthesis of polyfunctional 1,2,4-triazine systems bearing and/or containing phosphorus atoms as donor-acceptors interactions. Most of the synthetic methods depend on the interaction between an amino group of the side chain of 1,2,4-triazine with phosphorus reagents. The biological activities, i.e. their biocidal affects as antioxidants, antimicrobials, anti-inflammatory as well as molluscicidal agents against some snails are discussed.     

Die Acidität von Silanolgruppen. Vorläufige Mitteillung

The intrinsic acidity constant K_int. of surface silanol groups has been determined by coulometric titration of silicagel at 25° in solutions of the constant ionic strength 0,1M consisting primarily of sodium perchlorate. The experimental data are consistent with      

Evaluating formation and growth mechanisms of silica particles using fluorescence anisotropy decay analysis

At present, there is no direct experimental evidence that primary silica particles, which exist only transiently for a few seconds during the St?ber silica synthesis, can be stable in aqueous solutions. In the present work, we show that primary silica particles are formed spontaneously after the dissolution of diglycerylsilane (DGS) in aqueous solutions and remain stable for prolonged periods of time. By using time-resolved fluorescence anisotropy (TRFA), we demonstrate that this unique property of DGS is ascribed to the slow kinetics of silica particle growth in diluted sols at pH approximately 9.0. The anisotropy decay of the cationic dye rhodamine 6G (R6G), which strongly adsorbs to silica oligomers and nanoparticles in DGS sols, could be fit to three components: a fast (picosecond) scale component associated with free R6G, a slower (nanosecond) rotational component associated with R6G bound to primary silica particles, and a residual (nondecaying) anisotropy component associated with R6G that was bound to secondary or larger particles that were unable to rotate on the time scale of the R6G emission lifetime (4 ns). The data show that, under conditions where fast hydrolysis is obtained, the initial size of the nuclei depends on the silica concentration, with larger nuclei being present in more concentrated sols, while the rate of growth of primary particles depends on both silica concentration and solution pH. At low silica concentrations and high pHs, it was possible to observe the growth of stable, nonaggregating primary silica particles by a mechanism involving rapid nucleation followed by monomer addition. The presence of stable primary particles was confirmed by atomic force microscopy (AFM) imaging. At higher silica concentrations and lower pHs, there was an increase in the initial size of the nuclei formed, which subsequently grew to a larger radius (> 4.5 nm) or aggregated with time, and in such cases, nucleation and aggregation occurred simultaneously in the early stage of silica formation. The data clearly show the power of time-resolved fluorescence anisotropy decay measurements for probing the growth of silica colloids and show that this method is useful for elucidating the mechanism of particle formation and growth in situ.     

Chemo-enzymatic synthesis of 4-methylumbelliferyl beta-(1-->4)-D-xylooligosides: new substrates for beta-D-xylanase assays

Transglycosylation catalyzed by a beta-D-xylosidase from Aspergillus sp. was used to synthesize a set of 4-methylumbelliferyl (MU) beta-1-->4-D-xylooligosides having the common structure [beta-D-Xyl-(1-->4)]2-5-beta-D-Xyl-MU. MU xylobioside synthesized chemically by the condensation of protected MU beta-D-xylopyranoside with ethyl 2,3,4-tri-O-acetyl-1-thio-beta-D-xylopyranoside was used as a substrate for transglycosylation with the beta-D-xylosidase from Aspergillus sp. to produce higher MU xylooligosides. The structures of oligosaccharides obtained were established by 1H and 13C NMR spectroscopy and electrospray tandem mass spectrometry. MU beta-D-xylooligosides synthesized were tested as fluorogenic substrates for the GH-10 family beta-D-xylanase from Aspergillus orizae and the GH-11 family beta-D-xylanase I from Trichoderma reesei. Both xylanases released the aglycone from MU xylobioside and the corresponding trioside. With substrates having d.p. 4 and 5, the enzymes manifested endolytic activities, splitting off MU, MUX, and MUX2 primarily.     

Nets and generalized quadrangles

There is a new method of constructing generalized quadrangles (GQs) given by S. Löwe, which is based on covering of nets; all GQs with a regular point can be represented in this way. Here we give a method of constructing GQs with a regular point using the so-called content functions on nets. In the last part of the paper we lay the foundations for a research project aiming to use the more general notion of content to classify GQs and maybe to construct new ones.Both authors acknowledge the financial support by CRUI and DAAD in the frame of Programma Vigoni, which made this work possible.     

The first bis(orotato–N,O) complex: Synthesis,crystal structure,spectroscopic and thermal characterization of (chaH)2[Cu(HOr–N,O)2(cha)] · 2H2O (cha = cyclohexylamine and HOr = orotate(2−))

The novel bis(cyclohexylaminium) cyclohexylaminebis(orotate–N,O)cuprate(II) dihydrate, (C₆H₁₅N)₂[Cu(C₅H₂N₂O₄)₂(C₆H₁₄N)] · 2H₂O, has been prepared and characterized by elemental analysis, magnetic measurements, FT-IR and UV–Vis spectroscopy, thermal analysis and X-ray diffraction. The Cu(II) complex crystallizes in the monoclinic space group P2₁/c. The copper atom in the five-coordinated (chaH)₂[Cu(HOr–N,O)₂(cha)] · 2H₂O is chelated by a deprotonated pyrimidine nitrogen atom and carboxylate oxygen atom as a bis(bidentate) ligand and the cyclohexylamine ligand completes the square-pyramidal coordination. The thermal decomposition of the complex has been predicted by the help of thermal analysis (TG, DTG and DTA).     

Bimodal proton transfer in acid-base reactions in water

We investigate one of the fundamental reactions in solutions, the neutralization of an acid by a base. We use a photoacid, 8-hydroxy-1,3,6-trisulfonate-pyrene (HPTS; pyranine), which upon photoexcitation reacts with acetate under transfer of a deuteron (solvent: deuterated water). We analyze in detail the resulting bimodal reaction dynamics between the photoacid and the base, the first report on which was recently published. We have ascribed the bimodal proton-transfer dynamics to contributions from preformed hydrogen bonding complexes and from initially uncomplexed acid and base. We report on the observation of an additional (6 ps)(-1) contribution to the reaction rate constant. As before, we analyze the slower part of the reaction within the framework of the diffusion model and the fastest part by a static, sub-150 fs reaction rate. Adding the second static term considerably improves the overall modeling of the experimental results. It also allows to connect experimentally the diffusion controlled bimolecular reaction models as defined by Eigen-Weller and by Collins-Kimball. Our findings are in agreement with a three-stage mechanism for liquid phase intermolecular proton transfer: mutual diffusion of acid and base to form a "loose" encounter complex, followed by reorganization of the solvent shells and by "tightening" of the acid-base encounter complex. These rearrangements last a few picoseconds and enable a prompt proton transfer along the reaction coordinate, which occurs faster than our time resolution of 150 fs. Alternative models for the explanation of the slower "on-contact" reaction time of the loose encounter complex in terms of proton transmission through a von Grotthuss mechanism are also discussed.