Magnetic Core-Shell Nanoparticles Using Molecularly Imprinted Polymers for Zearalenone Determination

This paper describes the synthesis of novel molecularly imprinted magnetic nano-beads for the selective extraction (MISPE) of zearalenone mycotoxin in river and tap waters and further analysis by high-performance liquid chromatography (HPLC) with fluorescence detection (FLD). A semi-covalent imprinting approach was achieved for the synthesis of the molecularly imprinted polymers (MIP). The nanoparticles were prepared by covering the starting Fe₃O₄ material with a first layer of tetraethyl orthosilicate (TEOS) and then with a second layer using cyclododecyl 2-hydroxy-4-(3-triethoxysilylpropylcarbamoyloxy) benzoate. The last was used with a dual role, template and functional monomer after the extraction of the template molecule. The material was characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD) and Fourier transform infrared spectroscopies (FT-IR). The solid phase extraction was optimized in all the steps: loading, washing and elution. The optimal conditions allowed the determination of zearalenone in trace levels of 12.5, 25 and 50 µg L⁻¹ without significant differences between the fortified and found level concentrations.     

Synthesis, primary photophysical and antibacterial properties of naphthyl ester cinoxacin and nalidixic acid derivatives

We have synthesized two naphthyl ester quinolone derivates and determined their ability to generate reactive oxygen species (ROS) such as (1)O(2), ()OH, H(2)O(2) upon photolysis with UV-A light. The ability of cinoxacin (1) and nalidixic acid (2), and their naphthyl ester derivatives (3 and 4) to generate a dose-dependent amount of singlet oxygen and ROS (()(-)O(2), ()OH) in cell-free systems was detected by histidine assay and by luminol-enhanced chemiluminescence (LCL), respectively. Their electronic absorption and emission spectra were quantified and their photostability was determined. Their tendency to generate peroxidic derivative species showed the following order: 3>4; in contrast, their ability to generate singlet oxygen was 4>3 and these were better sensitizers than their parent quinolones 1 and 2. The antibacterial activity in darkness and under irradiation of compounds 3 and 4 was tested on Escherichia coli and compared with that of their parent compounds. An enhanced antibacterial activity by irradiation of the naphthyl esters of cinoxacin and nalidixic acid on E. coli was observed.     

Formation and analysis of particulate carbon in a synthetic lubricant

The formation of discrete carbonaceous particles has been investigated for a conventional synthetic ester-based lubricant degraded in thermal and thermal–oxidative environments. Experimental factors included oxidative and nonoxidative environments, high and low humidities, and the presence or lack of a metal catalyst surface, with all samples generated at 250 °C. Characterization performed for changes in antioxidant content, IR spectroscopy, molecular weight, total acid number, viscosity, and uv/vis absorbance spectrometry were used to determine the influences of the aforementioned variables on the rates of oil degradation and formation of high-molecular-weight species. Discrete carbonaceous particle formation was analyzed using Einstein's relationship for the viscoelastic behavior of particles in Newtonian fluids and by calculating associated radii of gyration. This viscoelastic behavior of the particles in solution is used to demonstrate how the absorption behavior of the carbonaceous degradation products tracks the discrete particulate species. The results show the formation of particulate species to be diffusion-limited after antioxidant depletion, and optical absorption analysis is shown to be a viable technique for monitoring the formation of discrete carbonaceous particles during lubricant degradation. Received: 29 February 2000/Accepted: 3 January 2000     

Purity determination as needed for the realisation of primary standards for elemental determination: status of international comparability

Within the National Metrology Institutes (NMIs) and designated laboratories, an interlaboratory comparison, CCQM-P107, was conducted to verify the degree of international comparability concerning the results of purity analysis. The mass fractions of Ag, Bi, Cd, Cr, Ni, Tl at the lower mg/kg-level in a high purity zinc material were determined, but the real measurand in metrological sense was the sum of the six mass fractions. Homogeneity was investigated by glow discharge mass spectrometry, reference values were obtained using isotope dilution mass spectrometry. Six NMIs participated, contributing eight independent data sets. The agreement amongst the results of the participants, their median and the agreement with the reference values were usually excellent and in almost all cases below the target uncertainty of 30% relative. In this manner, the accuracy of results and the comparability between the participants was demonstrated to be established.     

Effect of cryopreservation protocols on the phenotypic stability of yeast

Eight cryopreservation protocols were assessed for their effects on the viability and phenotypic stability of the yeast Saccharomyces cerevisiae during a five-year study. It is found that viability and phenotypic features have remained largely unchanged when the yeast was preserved in glycerol, dimethyl sulphoxide, or sucrose at -80 degrees C or in liquid nitrogen. When sorbitol was used as a cryoprotectant, yeast cells frozen and stored at -80 degrees C manifested great decreases in viability after six months in storage and concomitantly large fluctuations in the rate of the trpl auxotrophic reversion. This phenotypic reversion was stable passage after passage. Such a degree of phenotypic fluctuations, however, was not observed for yeast cells preserved in the same sorbitol solution that went through a controlled freezing program and were subsequently stored in liquid nitrogen. These results indicate that some combinations of cryoprotective agent, freezing program, and storage temperature disturb biomaterials more profoundly during cryopreservation and imply a genetic basis of this phenotypic change.     

Logic gates and elementary computing by enzymes

Different selected enzymes, glucose oxidase (GOx), catalase (Cat), glucose dehydrogenase (GDH), horseradish peroxidase (HRP), and formaldehyde dehydrogenase (FDH), are used alone or coupled to construct eight different logic gates. The added substrates for the respective enzymes, glucose and H(2)O(2), act as the gate inputs, while the biocatalytically generated gluconic acid or NADH are the output signals that follow the operation of the gates. Different enzyme-based gates are XOR, INHIBIT A, INHIBIT B, AND, OR, NOR, Identity and Inverter gates. By combining the AND and XOR or the XOR and INHIBIT A gates, the half-adder and half-subtractor are constructed, respectively, opening the way to elementary computing by the use of enzymes.     

Determination of thin film refractive index and thickness by means of film phase thickness

A new approach for determination of refractive index dispersion n(λ) (the real part of the complex refractive index) and thickness d of thin films of negligible absorption and weak dispersion is proposed. The calculation procedure is based on determination of the phase thickness of the film in the spectral region of measured transmittance data. All points of measured spectra are included in the calculations. Barium titanate thin films are investigated in the spectral region 0.38–0.78 μm and their n(λ) and d are calculated. The approach is validated using Swanepoel’s method and it is found to be applicable for relatively thin films when measured transmittance spectra have one minimum and one maximum only.      

Synthesis,characterization and biological activities of <Emphasis Type=Italic>N</Emphasis>-heteroaromatic hydrazones and their complexes with Pd(II), Pt(II) and Cd(II)

Condensation derivatives of ethyl hydrazinoacetate with 2-formylpyridine and quinoline-2-carboxaldehyde were synthesized. Pd(II), Pt(II) and Cd(II) complexes with the 2-formylpyridine derivative and a Cd(II) complex with the quinoline-2-carboxaldehyde derivative were synthesized and characterized by spectroscopic techniques. In the complexes, both ligands are coordinated in neutral NN bidentate modes, while the remaining two coordination sites are occupied by chloride. All compounds showed biological activity when tested against Escherichia coli, Bacillus subtilis and Staphylococcus aureus.     

A dynamic soil chamber system coupled with a tunable diode laser for online measurements of δ13C, δ18O,and efflux rate of soil‐respired CO2

High frequency observations of the stable isotopic composition of CO₂ effluxes from soil have been sparse due in part to measurement challenges. We have developed an open‐system method that utilizes a flow‐through chamber coupled to a tunable diode laser (TDL) to quantify the rate of soil CO₂ efflux and its δ¹³C and δ¹⁸O values (δ¹³C_R and δ¹⁸O_R, respectively). We tested the method first in the laboratory using an artificial soil test column and then in a semi‐arid woodland. We found that the CO₂ efflux rates of 1.2 to 7.3 µmol m^?2 s^?1 measured by the chamber‐TDL system were similar to measurements made using the chamber and an infrared gas analyzer (IRGA) (R² = 0.99) and compared well with efflux rates generated from the soil test column (R² = 0.94). Measured δ¹³C and δ¹⁸O values of CO₂ efflux using the chamber‐TDL system at 2 min intervals were not significantly different from source air values across all efflux rates after accounting for diffusive enrichment. Field measurements during drought demonstrated a strong dependency of CO₂ efflux and isotopic composition on soil water content. Addition of water to the soil beneath the chamber resulted in average changes of +6.9 µmol m^?2 s^?1, ?5.0‰, and ?55.0‰ for soil CO₂ efflux, δ¹³C_R and δ¹⁸O_R, respectively. All three variables initiated responses within 2 min of water addition, with peak responses observed within 10 min for isotopes and 20 min for efflux. The observed δ¹⁸O_R was more enriched than predicted from temperature‐dependent H₂O‐CO₂ equilibration theory, similar to other recent observations of δ¹⁸O_R from dry soils (Wingate L, Seibt U, Maseyk K, Ogee J, Almeida P, Yakir D, Pereira JS, Mencuccini M. Global Change Biol. 2008; 14: 2178). The soil chamber coupled with the TDL was found to be an effective method for capturing soil CO₂ efflux and its stable isotope composition at high temporal frequency. Published in 2010 by John Wiley & Sons, Ltd.