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.     

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.     

Experimental and Theoretical Study on the Inclusion Capability of a Fluorescent Indolizine β-Cyclodextrin Sensor Towards Volatile and Semi-volatile Organic Guest

Inclusion equilibria of a new fluorescent indolizine modified β-cyclodextrin were studied in aqueous solution to evaluate its use as a fluorescent chemo-sensor for volatile organic compounds (VOCs). The host compound shows a decrease of the fluorescence intensity by adding adamantanol, benzene, toluene, phenol and p-cresol as guest. The sensing parameter (ΔI/I ₀) was used to show the sensing ability of the host. The formation constant values measured using a spectral displacement method and a specific algorithm treatment are reported. Although the guest binding ability of the sensor is not enhanced by the existence of the hydrophobic cap, this new cyclodextrin sensor shows a very strong sensing ability. The experimental values of the constants were in good agreement with the computed complexation energies, ΔE, from molecular mechanics modelling of the inclusion process.