Determination of zeranol and beta-zearalanol in calf urine by immunoaffinity extraction and gas chromatography-mass spectrometry after repeated administration of zeranol

A method for the determination of zeranol and its metabolite beta-zearalanol in bovine urine is described. It has been applied to samples from calves given multiple subcutaneous doses of zeranol. Samples were extracted with immunoaffinity columns containing antibodies raised against zeranol and were analysed by gas chromatography-mass spectrometry. The immunoaffinity columns were prepared by coupling immunoglobulin G fractions obtained from rabbit antisera with a Sepharose matrix. The immunizing agent was carboxybutylzeranol coupled to bovine serum albumin. Gas chromatography-mass spectrometry was performed in the negative-ion chemical ionization mode, after derivatization of the compounds to their pentafluorobenzyl ethers, and allowed detection of analytes with a sensitivity of 0.01 ppb in spiked urine. The derivatization method and the gas chromatographic determination were also applied to the similar compounds zearalanone, zearalenone and beta-zearalenol. A synthesis of dideuterated zeranol and beta-zearalanol by isotopic exchange is described. These deuterated analogues had an isotopic purity of more than 99% and were used for quantitation of zeranol and beta-zearalanol by isotope dilution mass spectrometry. The recoveries of zeranol and beta-zearalanol, using the immunoaffinity columns, were determined after extraction from spiked urine and were 84 and 64%, respectively. The urines of treated calves were collected for several days after treatments and were analysed after hydrolysis with beta-glucuronidase and arylsulphatase. The samples showed variable but generally decreasing concentrations of zeranol and beta-zearalanol. The levels of beta-zearalanol ranged from less than 0.01 to 98 ppb and were 1.2-3.2 times higher than those of zeranol.     

A new instrument for time-resolved reduction of scattered radiation in fluorescence measurements

An opto-electronic cross-correlation system was employed to reduce the scattering influence in fluorescence measurements. A stable optical delay line incorporated into the instrument was positioned to yield detection at a fixed time after excitation; the optimal delay time was determined simply from the ratio of the fluorescence decay curve to a similar curve portraying scattering response. Signal-to-scattering background enhancements greater than two were measured for the very short-lived (τ = 0.7 ns) fluorophores whereas a six-fold increase was measured for fluorophores with longer lifetimes. The shortest lifetime which would benefit from time-resolution in this system is limited by the time-response of the photomultiplier tube (1.1 ns FWHM); the excitation pulses are on the order of 6 ps.     

The boundedness of the Cauchy singular integral operator in weighted Besov type spaces with uniform norms

The mapping properties of the Cauchy singular integral operator with constant coefficients are studied in couples of spaces equipped with weighted uniform norms. Recently weighted Besov type spaces got more and more interest in approximation theory and, in particular, in the numerical analysis of polynomial approximation methods for Cauchy singular integral equations on an interval. In a scale of pairs of weighted Besov spaces the authors state the boundedness and the invertibility of the Cauchy singular integral operator. Such result was not expected for a long time and it will affect further investigations essentially. The technique of the paper is based on properties of the de la Vallée Poussin operator constructed with respect to some Jacobi polynomials.     

Introduction to Session 4

Applied Biochemistry and Biotechnology -     

YBCO step-edge SQUIDs by magnetron sputtering technique

Summary YBCO step-edge junction d.c. SQUIDs have been realized by using the Inverted Cylindrical Magnetron Sputtering (ICMS) technique. This last represents a novel technology for high-T _c Josephson junctions (HTSC). Steps are obtained by standard ion milling procedure on LaAlO₃ (100) substrates using Nb-masks patterned by reactive ion etching. Measurements of currentvs. voltage, maximum d.c. Josephson currentvs. magnetic field and SQUID voltage response measurements have been performed, also as a function of the temperature. Operating temperature as high as 77K has been achieved. At 4.2K the SQUIDs show a maximum voltage of flux transfer function (∂V/∂ϕ)_max=870 μV/Ф₀ and a good periodicity of theV-ϕ modulation up to 20Ф₀ without any sign of hysteresis. The ratio between the step height (h) and the film thickness (d) seems to play a fundamental role in determining Josephson properties of the bridges, these conditions being more severe with respect to most of the data available in literature. Paper presented at the ?VII Congresso SATT?, Torino, 4–7 October 1994.     

Structural investigation of YBCO films and bicrystal grain boundary junctions

Summary We present a structural analysis of YBCO superconducting thin films fabricatedin situ by Inverted Cylindrical Magnetron (ICM) sputtering on commercial SrTiO₃ single-crystal and bicrystal substrates. A detailed structural characterization of the superconductor films was performed by using single-crystal X-ray diffractometry confirming that YBCO films have a strongc-axis orientation of the grains with a small mosaic spread. In the films grown on bicrystal substrates we observed a strong correlation with the lattice structure of the substrate. In addition, a surface analysis of the region across the grain boundary edge has been performed by using scanning electron microscopy. Paper presented at the ?VII Congresso SATT?, Torino, 4–7 October 1994.     

Transition states and energy barriers from density functional studies: Representative isomerization reactions

Three representative isomerization reactions (HNC → HCN, CH₃NC → CH₃CN, and N₂H₂ trans → cis and sin) have been studied using both the LCGTO–LSD and LCGTO–NLSD density functional methods and employing a new algorithm for the search and the refinement of the transition-state structures. The inclusion of the nonlocal corrections and the use of large basis sets improve the reliability of the energetic parameters. Results are in good agreement with previous accurate first-principle computations and available experimental data. © John Wiley & Sons, Inc.