Retention Behavior of New Oral Antidiabetic Drugs in Reversed-Phase Chromatography

JPC – Journal of Planar Chromatography – Modern TLC - The thin-layer chromatographic behavior of three of the newest oral antidiabetic agents, pioglitazone, rosiglitazone, and...     

Do intramolecular halogen bonds exist? Ab initio calculations and crystal structures’ evidences

Cl···O intramolecular contacts are analysed here. Hence the Cambridge Structural Database (CSD) search was performed to find five-membered Cl–C=C–C=O pseudo-rings closed through Cl···O intramolecular contacts. Such rings were analysed and it was found that some of Cl···O distances are smaller than the corresponding sum of van der Waals radii. Additionally ab initio MP2/6-311++G(d,p) calculations and AIM analyses were carried out here on 3-chloropropenal and its fluoro derivatives to deepen the nature of intramolecular Cl···O interactions, some of findings may indicate that they are attractive and stabilizing ones. This paper is dedicated to Prof. T. M. Krygowski on the occasion of his 70th birthday     

Solvation force for long-ranged wall--fluid potentials

The solvation force of a simple fluid confined between identical planar walls is studied in two model systems with short ranged fluid-fluid interactions and long-ranged wall-fluid potentials decaying as -Az(-p),z--> infinity, for various values of p. Results for the Ising spins system are obtained in two dimensions at vanishing bulk magnetic field h=0 by means of the density-matrix renormalization-group method; results for the truncated Lennard-Jones (LJ) fluid are obtained within the nonlocal density functional theory. At low temperatures the solvation force f(solv) for the Ising film is repulsive and decays for large wall separations L in the same fashion as the boundary field f(solv) approximately L(-p), whereas for temperatures larger than the bulk critical temperature f(solv) is attractive and the asymptotic decay is f(solv) approximately L(-(p+1)). For the LJ fluid system f(solv) is always repulsive away from the critical region and decays for large L with the the same power law as the wall-fluid potential. We discuss the influence of the critical Casimir effect and of capillary condensation on the behavior of the solvation force.     

Synthesis of macrocyclic tetraamides derived from α-amino acids and their investigations using ESI-MS technique

Chiral α,ω-diesters react under high-pressure conditions (10 kbar) with α,ω-diamines to give chiral cyclic tetraamides of C₂-symmetry. The complexation properties of tetraamides towards alkali metal cations (Li⁺, Na⁺, K⁺, Rb⁺ and Cs⁺) were estimated on the basis of ESI-MS spectra.     

Evaluation of a purge-and-trap injection system for capillary gas chromatography-microwave induced plasma-atomic emission spectrometry for the determination of volatile selenium compounds in water

A method is presented for the selective determination of the volatile selenium species dimethylselenide and dimethyldiselenide, using a commercially available purge-and-trap injection system coupled to capillary gas chromatography-microwave induced plasma-atomic emission spectrometry. The efficiency of the purging step was evaluated and the parameters affecting the purge and trap processes were optimized. The method was applied to the determination of volatile selenium compounds in lake water. Relative detection limits of 2ng/l for dimethylselenide and dimethyldiselenide, corresponding to an absolute detection limit of 10 pg, were achieved.     

Thiol-ene chemistry as an effective tool for hydrophobization of cotton fabrics

In this paper, several methods of hydrophobization of cotton fabrics using the thio-ene click reaction were compared. Durable, superhydrophobic textiles were obtained in an easy way. Various variants of functionalized silsesquioxanes were used for the hydrophobization of fabrics. The synthesis of bifunctional silsesquioxanes (RSiMe₂O)₄(ViSiMe₂O)₄Si₈O₁₂ and (RSiMe₂O)₄(R’SiMe₂O)₄Si₈O₁₂ were performed via hydrothiolation of silsesquioxane derivative (ViSiMe₂O)₈Si₈O₁₂. Alkoxysilyl, alkyl and fluoroalkyl moieties were introduced as functional groups. Samples were prepared using four methods, differing in the modification method and the number of stages. During the research, fabrics were modified via (a) the dip-coating process, (b) carrying out thiol-ene click reactions directly on the surface of the fabric and (c) using both of these methods. The hydrophobicity of the fabric was evaluated by measuring the Water contact angle (WCA). The obtained samples were also examined using infrared analysis (FT-IR), Scanning electron microscope (SEM), and Elemental analysis (SEM–EDS). All analyses were performed before and after the washing process in order to verify the stability of the performed modifications.

Graphical abstract

     

Electrooxidation of phenol at exfoliated graphite electrode in alkaline solution

The present paper reports on exfoliated graphite (EG) used for the cyclic electrochemical process of phenol oxidation in alkaline solution. It is shown that the electrochemical activity of anode-produced EG decreases considerably in the second cycle due to the deposition of an oligomer film, composed of the products of phenol oxidation, on the EG surface. Thermal treatment of the inactive graphite anode in air at 500 °C provided a regenerated material of activity three times higher for the first cycle and 2.6 times higher for three cycles as compared to the original anode. The reason for such a behavior is assigned to a carbon film formed on the EG surface during the carbonization/oxidation processes involving the products of phenol oxidation. Comparative studies showed that electroactivity of the original EG can also be enhanced if before the process of phenol oxidation the original EG is activated by heat treatment. Unfortunately, the electrochemical activity of the product of such a treatment is higher only for the first cycle of phenol oxidation and drops dramatically in the following cycles.Contribution to the 3rd Baltic Conference on Electrochemistry, Gdask-Sobieszewo, 23–26 April 2003. Dedicated to the memory of Harry B. Mark, Jr. (28 February 1934–3 March 2003)     

Copolymer of Di (methacryloyloxymethyl) naphthalene and divinylbenzene as a column packing for high-performance liquid chromatography

Summary A new porous polyaromatic ester packing was synthetized for high performance liquid chromatography. The relationship between retention and chain length of the members of homologous series of alkylbenzenes, N-alkylanilines, alkylarylethers, alkylbenzoates and alkylarylketones on this new stationary phase using different eluents was investigated. Using the alkylarylketone scale the retention indices of the homologues and test compounds were calculated. The results were compared with those obtained for poly (styrene-divinylbenzene) polymers. For both types of packing the first members of each homologous series gave non-linear behaviour. The methylene group index increments are different for the studied homologous series; thus there is no simple additivity of the retention indices. The efficiency of the porous polymeric columns is a function of the capacity factor of the solute and the organic component of the eluent.     

Luminescence Properties of Tb-Doped Yttrium Disilicate Prepared by the Sol–Gel Method

A sol–gel method for the synthesis of nanosized powders of yttrium disilicate doped with Tb^{3 +} is presented. The influence of grain size and annealing temperature on the structure and luminescence properties of the materials obtained has been investigated. The preparation of glass-ceramic composite has been also described. The effect of incorporating the nanocrystals into sol–gel silica glasses on their physicochemical properties has been shown and discussed. A lack of influence of the annealing above 1300°C on the lifetimes measured for the nanocrystals embedded in the glass, as compared to the Y₂Si₂O₇:Tb^{3 +} powders, has been observed.     

Insights into the structure of cyclohexane from femtosecond degenerate four-wave mixing spectroscopy and ab initio calculations

In this paper, we report the use of femtosecond time-resolved degenerate four-wave mixing rotationally resolved spectroscopy to obtain very accurate structural information on the symmetric top cyclohexane. Apart from highlighting the versatility of this method in determining accurate structures of large and complex molecules without dipole moment, the present study also details the comparison of the experimentally determined rotational constant B(0) with that obtained from high-level ab initio calculations. The theoretical calculations, which were carried out at both the second-order M?ller-Plesset (MP2) and coupled-cluster with single, double, and perturbative triple substitutions [CCSD(T)] levels of theory, also take into account vibrational averaging effects. A detailed investigation of the vibrational averaging effects reveals that the corrections emerge from only the six highly symmetric A(1g) modes, a justification of which is provided by an analysis of these modes.