Electrodeposition of mercury film on electrodes modified with clay minerals

A new type of carbon paste electrode modified with clay mineral and covered with a mercury film is presented in this work. Electrodeposition of the mercury film was performed on the carbon paste electrode modified with montmorillonite. The mercury film was deposited by both electrodeposition in situ and a preliminary electrodeposition. The pre-deposited film of mercury showed to be suitable for anodic stripping voltammetry. An open-circuit sorption of Cd, Pb, and Cu with subsequent anodic stripping voltammetry exhibited higher current responses of metals. Besides the enhanced sensitivity superior separation of the current responses during a simultaneous stripping of metals is expected to be achieved by means of the newly prepared electrode. Presented at the 57th Congress of Chemical Societies, Tatranské Matliare, 4–8 September 2005.     

A comparison of performance of various analytical columns in pharmaceutical analysis: conventional C18 and high throughput C18 zorbax columns

New improved types of analytical columns Zorbax Eclipse XDB-C18 (75 mm x 4.6 mm i.d., 3.5 microm) and Zorbax Eclipse XDB-C18 (50 mm x 4.6 mm i.d., 1.8 microm) have been tested for determination of estradiol (active substance), methylparaben, propylparaben (preservatives) and estrone (degradation product) and compared with the conventional C18 columns (250 mm x 3.0 mm i.d., 5.0 microm). The Zorbax columns differ with their particle size, column length and ODS (octadecylsilica) type as well. Higher flow-rates (up to about 2.5 ml min(-1)) could be applied regardless to back-pressure. The analysis - previously done at 40 degrees C - could be performed even at ambient temperature. Analytical run was shortened to 3.5 min (from 12 min used for the conventional C18 column) with the same or better retention characteristics. System suitability data for all Zorbax columns show the advantages of these columns for the practical use in routine quality control of pharmaceuticals, particularly from the point of view of speed of analysis and solvent consumption.     

Biocompatible hydrogels based on chitosan,cellulose/starch,PVA and PEDOT:PSS with high flexibility and high mechanical strength

Fabricating mechanically strong hydrogels that can withstand the conditions in internal tissues is a challenging task. We have designed hydrogels based on multicomponent systems by combining chitosan, starch/cellulose, PVA, and PEDOT:PSS via one-pot synthesis. The starch-based hydrogels were homogeneous, while the cellulose-based hydrogels showed the presence of cellulose micro- and nanofibers. The cellulose-based hydrogels demonstrated a swelling ratio between 121 and 156%, while the starch-based hydrogels showed higher values, from 234 to 280%. Tensile tests indicated that the presence of starch in the hydrogels provided high flexibility (strain at break?>?300%), while combination with cellulose led to the formation of stiffer hydrogels (elastic moduli 3.9–6.6 MPa). The ultimate tensile strength for both types of hydrogels was similar (2.8–3.9 MPa). The adhesion and growth of human osteoblast-like SAOS-2 cells was higher on hydrogels with cellulose than on hydrogels with starch, and was higher on hydrogels with PEDOT:PSS than on hydrogels without this polymer. The metabolic activity of cells cultivated for 3 days in the hydrogel infusions indicated that no acutely toxic compounds were released. This is promising for further possible applications of these hydrogels in tissue engineering or in wound dressings.

Graphical abstract

     

RP-HPLC analysis of phenolic compounds and flavonoids in beverages and plant extracts using a CoulArray detector

Methods were developed for the analysis of natural antioxidants including phenolic compounds and flavonoids in beverages and plant extracts using gradient HPLC with multi-channel electrochemical coulometric detection. Suitability of various reversed-phase columns for this purpose was compared; pH and mobile phase gradients were optimized with respect to the separation selectivity and sensitivity of detection. Because of different target compounds in various sample types, the overlapping resolution maps and the normalized resolution product approaches described earlier were used to select optimum columns and gradients to suit the analysis of the individual sample types. The methods were applied to the analysis of phenolic compounds and flavonoids in beer, wine, tea, and yacon extracts. 32 phenolic compounds were identified and determined, including derivatives of benzoic and cinnamic acids, flavones, and a few related glycosides. Eight-channel CoulArray detection offers high selectivity and sensitivity with limits of detection in the low microg L(-1) range, at least an order of magnitude lower than single-channel coulometric detection using the Coulochem detector. No special sample pretreatment is necessary and, because of the compatibility of the CoulArray detector with gradient elution, phenolic antioxidants of different polarities can be determined in a single run. In addition to the retention times, the ratios of the areas of the pre-dominant and post-dominant peaks to the area of the dominant peak can be used for improved identification of natural antioxidants.     

Internal friction in cd+zn alloy single crystals

Internal friction measurements were used for the examination of Cd + Zn alloy single crystals. It was established that the interaction energy between solute Zn atoms and dislocations in basal planes is 0·12 eV.The authors thank Dr. P.Luká, CSc., for valuable discussions.     

A New Insight into the Stereoelectronic Control of the Pd0-Catalyzed Allylic Substitution: Application for the Synthesis of Multisubstituted Pyran-2-ones via an Unusual 1,3-Transposition

Pyran-2-ones 3 undergo a novel Pd⁰-catalyzed 1,3-rearrangement to afford isomers 6 . The reaction proceeds via an η²-Pd complex, the pyramidalization of which (confirmed by quantum chemistry calculations) offers a favorable antiperiplanar alignment of the Pd−C and allylic C−O bonds ( C ), thus allowing the formation of an η³-Pd intermediate. Subsequent rotation and rate-limiting recombination with the carboxylate arm then gives isomeric pyran-2-ones 6 . The calculated free energies reproduce the observed kinetics semi-quantitatively.     

Development and optimization of ultra-high performance supercritical fluid chromatography mass spectrometry method for high-throughput determination of tocopherols and tocotrienols in human serum

The goal of this study was to develop an effective supercritical fluid chromatography method using single quadrupole MS for analysis of all isomeric forms of vitamin E. Finally, two fast and effective methods, the high resolution one and the high speed one, for the determination of 8 vitamin E isomers in human serum were developed.     

Non‐thermal plasma‐induced apoptosis in yeast Saccharomyces cerevisiae

The effect of non‐thermal plasma generated by the direct current (DC) corona discharge in the mode of transition spark is studied on a yeast Saccharomyces cerevisiae. The exposure to plasma increases production of reactive oxygen species (ROS) in cells, possibly causing the induction of apoptosis. To clarify the mechanism of apoptosis, its induction is tested not only on a wild strain of S. cerevisiae, but also on mutant strains: A deletion mutant Δyca1 without yeast metacaspase proves that in S. cerevisiae the apoptosis occurs partly by the caspase‐independent pathway. A petite strains with mutation in the mitochondria do not show pronounced ROS formation, but in spite of this, apoptosis is detected. Hence, mitochondrial ROS probably do not play an important role in induction of apoptosis.