Interdisciplinary study on pottery experimentally impregnated with wine

Experimentally developed ceramic pots, with two different sizes of grain, were half-filled with wine and subjected to thermal alteration at constant elevated temperature ((60 ± 2)°C) in darkness for 12 weeks. This work sought to characterise the samples thereby obtained from chemical and mineralogical perspectives using scanning electron microscopy and an energy-dispersive X-ray microanalysis system (SEM-EDX), Fourier transform infrared spectroscopy (FTIR) and capillary electrophoresis (CE) with UV detection as an alternative to chromatographic methods, due to its good resolution, automation, simplicity, high speed, low consumption of chemicals and short time required for sample preparation. The capillary electrophoresis method was used for the detection of five wine biomarkers: succinic acid, malic acid, tartaric acid, citric acid and lactic acid. In general, it was noted that the fine-grained ceramic assortment retained the organic material better than the coarser-grained ceramics. An interesting observation derived from this study was that not only could tartaric acid be considered as a biomarker for wine residues in archaeological pottery, but malic acid could also act similarly for white wine and lactic acid for red wine.     

The effect of the hydration degree on the hydrothermal and thermo-oxidative stability of some collageneous matrices

The methods of the thermal analysis (TG, DTG and DTA) were used in order to investigate the effect of the hydration degree on the thermal behaviour of some collageneous matrices. It was pointed out that the degradation of hydrated collagen in the temperature range 20-400°C occurs through two successive processes accompanied by mass losses. The first process, consisting in the collagen dehydration, is endothermic and takes place in the temperature range ≈25 - ≈125°C. The second process is exothermic and consists in the decomposition and/or thermo-oxidation of dry collagen. The thermal parameters of both processes depend on the hydration degree of collagen. The observed dependencies show that the hydrothermal and thermo-oxidative stability of collagen are strongly correlated with its water content. This revised version was published online in July 2006 with corrections to the Cover Date.     

Development of an enzymatic microreactor based on microencapsulated laccase with off-line capillary electrophoresis for measurement of oxidation reactions

Microencapsulation is used here as a new technique to immobilize enzymes in a microreactor coupled off-line to capillary electrophoresis (CE), allowing the determination of enzymatic reaction products. The redox enzyme laccase was encapsulated using the method of interfacial cross-linking of poly(ethyleneimine) (PEI). The 50 μm diameter capsules were slurry packed from a suspension into a capillary-sized reactor made easily and quickly from a short length of 530 μm diameter fused-silica tubing. The volume of the bed of laccase microcapsules in the microreactor was in the order of 1.1 μL through which 50 μL of the substrate o-phenylenediamine (OPD) was flowed. The oxidation product 2,3-diaminophenazine (DAP) and the remaining OPD were quantified by CE in a pH 2.5 phosphate buffer. Peak migration time reproducibility was in the order of 0.4% RSD and peak area reproducibility was less than 1.7% RSD within the same day. Using the OPD peak area calibration curve, a conversion efficiency of 48% was achieved for a 2-min oxidation reaction in the microreactor.     

Conformational Study of Glycal-Type Neuraminidase Inhibitors

The conformational flexibility of two glycal-type neuraminidase inhibitors has been studied, using several molecular modeling techniques. In agreement with the experimental data available, an intramolecular hydrogen bond, representing a key structural feature that controls the conformer distribution in solution, has been identified. The contribution of each substituent to the overall equilibrium was evaluated using simplified derivatives. Additionally, four methods for estimating NMR coupling constants from dihedral angles were evaluated and the Haasnoot method was found to be appropriate for this class of sugars. These results should allow a better understanding of the structural parameters governing physico-chemical properties of glycal-like compounds. Supplemental materials are available for this article. Go to the publisher's online edition of Journal of Carbohydrate Chemistry to view the free supplemental file.     

Rare earth doped cobalt ferrite thin films deposited by PLD

CoFe₂O₄ thin films with preferential texture structure, small grain size, and perpendicular magnetic anisotropy can be obtained by the pulsed laser deposition (PLD) technique. In this work, we studied the influence of the Fe³⁺ ions substitution by three elements from lanthanide group (Dy, La, and Gd) on the structural properties of the thin films. The samples were deposited by Nd:YAG laser (λ=532 nm, 10 ns) ablation of CoFe_1.8RE_0.2O₄, (RE=Dy, La, Gd) targets at various substrate temperatures ranging from room temperature to 600 °C. The microstructure and chemical composition of the thin films were investigated by Raman spectroscopy, XRD, SEM-EDS, and ToF-SIMS. The XRD patterns and Raman spectra of the thin films indicated the formation of a single spinel structure. Thus, the desired substitution of the iron ions in the spinel lattice with the RE elements was achieved in the thin films, although in the bulk material, their presence determined the formation of a residual phase with a perovskite-type structure.     

Measurement of the sputter yield after mild ion erosion of a pristine Cu(001) surface

Using the STM technique we have determined the sputter yield on a pristine Cu(001) surface after mild (fluence less than 0.044 ions per surface atom) bombardment of the pristine surface with 800 eV Ar⁺ions at normal incidence. The experiments have been performed at substrate temperatures ranging from 200 to 350 K. Making use of the positional correlation of adatoms and surface vacancies, at 200 K and 325 K, we concluded that about 1/3 of the surface adatoms originate from interstitials arriving at the surface and they give a direct indication of the buried bulk vacancies. A careful analysis of the different areas for surface vacancies and adatom then allowed a quantitative evaluation of the sputter yield at 1.2 Cu atoms per 800 eV Ar⁺ ion.     

A Comparative Loading and Release Study of Vancomycin from a Green Mesoporous Silica

Since its first use as a drug delivery system, mesoporous silica has proven to be a surprisingly efficient vehicle due to its porous structure. Unfortunately, most synthesis methods are based on using large amounts of surfactants, which are then removed by solvent extraction or heat treatment, leading to an undesired environmental impact because of the generated by-products. Hence, in the present study, we followed the synthesis of a silica material with a wormhole-like pore arrangement, using two FDA-approved substances as templates, namely Tween-20 and starch. As far as we know, it is the first study using the Tween-20/starch combo as a template for mesoporous silica synthesis. Furthermore, we investigated whether the obtained material using this novel synthesis had any potential in using it as a DDS. The material was further analyzed by XRD, TEM, FT-IR, N₂ adsorption/desorption, and DLS to investigate its physicochemical features. Vancomycin was selected as the active molecule based on the extensive research engaged towards improving its bioavailability for oral delivery. The drug was loaded onto the material by using three different approaches, assuming its full retention in the final system. Thermal analysis confirmed the successful loading of vancomycin by all means, and pore volume significantly decreased upon loading, especially in the case of the vacuum-assisted method. All methods showed a slower release rate compared to the same amount of the pure drug. Loadings by physical mixing and solvent evaporation released the whole amount of the drug in 140 min, and the material loaded by the vacuum-assisted method released only 68.2% over the same period of time, leading us to conclude that vancomycin was adsorbed deeper inside the pores. The kinetic release of the three systems followed the Higuchi model for the samples loaded by physical mixing and vacuum-assisted procedures, while the solvent evaporation loading method was in compliance with the first-order model.     

Attempts to Access a Series of Pyrazoles Lead to New Hydrazones with Antifungal Potential against Candida species including Azole-Resistant Strains

The treatment of benzylidenemalononitriles with phenylhydrazines in refluxing ethanol did not provide pyrazole derivatives, but instead furnished hydrazones. The structure of hydrazones was secured by X-ray analysis. The chemical proof was also obtained by direct reaction of 3,4,5-trimethoxybenzaldehyde with 2,4-dichlorophenylhydrazine. Newly synthesized hydrazones were tested against eight Candida spp. strains in a dose response assay to determine the minimum inhibitory concentration (MIC₉₉). Five compounds were identified as promising antifungal agents against Candida spp. (C. albicans SC5314, C. glabrata, C. tropicalis, C. parapsilosis and C. glabrata (R azoles)), with MIC₉₉ values ranging from 16 to 32 µg/mL and selective antifungal activity over cytotoxicity.