Quantitative analysis of oxytetracycline and its 4-epimer in calf tissues by high-performance liquid chromatography combined with positive electrospray ionization mass spectrometry

Tetracycline antibiotics are commonly used in veterinary medicine because of their broad spectrum activity and cost effectiveness. Oxytetracycline (OTC) is one of the most important members of this antibiotic family. The purpose of this study was to develop and validate a method to determine OTC residues in edible tissues of calf. Extraction of OTC and its 4-epimer (4-epiOTC), in the presence of the internal standard demethylchlortetracycline (DMCTC), was performed using a liquid extraction with sodium succinate solution (pH 4.0), followed by protein removal with trichloroacetic acid and paper filtration. Further solid-phase extraction clean-up on an HLB polymeric reversed phase column was performed to obtain an extract suitable for LC-MS-MS analysis. Chromatographic separation of the internal standard, and especially OTC and its 4-epimer, was achieved on a PLRP-S polymeric reversed phase column, using a mixture of 0.001 M of oxalic acid, 0.5% (v/v) of formic acid and 3% (v/v) of tetrahydrofuran in water (mobile phase A) and tetrahydrofuran (mobile phase B) as the mobile phase, and at a column temperature of 60 degrees C. OTC and its 4-epimer could be identified using the MS-MS detection technique, and were subsequently quantified. The method has been validated according to the requirements of the EC at the MRL (maximum residue limit, 100 ng g(-1) for muscle, 300 ng g(-1) for liver and600 ng g(-1) for kidney), half the MRL and double the MRL levels, as well for OTC as for 4-epiOTC. Calibration graphs were prepared for all tissues and good linearity was achieved over the concentration ranges tested (r > 0.99 and goodness of fit < 10%). Limits of quantification of half the MRLs were obtained for the analysis of OTC and 4-epiOTC in muscle, liver and kidney tissues of calf. Limits of detection ranged for both components between 0.8 and 48.2 ng g(-1). The within-day and between-day precisions, expressed as RSD values, were all below the maximum allowed RSD values calculated according to the Horwitz equation. The results for accuracy fell within the -20% to +10% range. Recoveries were between 47 and 56% for OTC, and between 52 and 62% for 4-epiOTC, depending on the tissue. The method has been successfully used for the quantitative determination of OTC and 4-epiOTC in tissue samples of calves medicated with OTC by intramuscular injection.     

Comparison of different fibers for the solid-phase microextraction of phthalate esters from water

Solid-phase microextraction (SPME) coupled to gas chromatography-mass spectrometry (GC-MS) has been applied to determine six phthalate esters and one adipate ester in water. The SPME parameters were optimized for several commercially available fibers. A 65-microm polydimethylsiloxane-divinylbenzene (PDMS-DVB) was the fiber selected and was applied to analysis of water from the Ebro river and the industrial port of Tarragona. The studied compounds were found at concentrations ranging from 0.4 microg l(-1) for di-n-butyl phthalate ester (DnBP) to 3.2 microg l(-1) for bis(2-ethylhexyl) phthalate ester (DEHP). The linear range for real samples was from 0.1 to 10 microg l(-1) for most phthalates, and the limits of detection of the method were between 3 and 30 ng l(-1). Repeatability and reproducibility between days (n = 5) for 1 microg l(-1) samples were below 13 and 18%, respectively.     

A note on the Holst action, the time gauge, and the Barbero–Immirzi parameter

In this note, we review the canonical analysis of the Holst action in the time gauge, with a special emphasis on the Hamiltonian equations of motion and the fixation of the Lagrange multipliers. This enables us to identify at the Hamiltonian level the various components of the covariant torsion tensor, which have to be vanishing in order for the classical theory not to depend upon the Barbero–Immirzi parameter. We also introduce a formulation of three-dimensional gravity with an explicit phase space dependency on the Barbero–Immirzi parameter as a potential way to investigate its fate and relevance in the quantum theory.     

Study of the retention behavior of iodinated X‐ray contrast agents in hydrophilic interaction liquid chromatography,comparing bare silica and zwitterionic stationary phases

Iodinated X‐ray contrast media are the most widely used pharmaceuticals for intravascular administration in X‐ray diagnostic procedures. The increasing concern of the fate of these compounds into the environment has led to the development of analytical methods to determine them. However, these methods present problems due to the polar character of these analytes. In this paper, hydrophilic interaction LC is presented as an alternative technique. The retention of iodinated X‐ray contrast media was studied in two bare silica phases with different particle designs (i.e. porous and Fused Core?) and a zwitterionic sulfoalkylbetaine phase. The effect of the most important parameters of the mobile phase was studied for each stationary phase. It was observed that optimal mobile phase conditions included buffers with a high buffering capacity. Additionally, the retention mechanisms involved were studied in order to provide some insight into the possible occurring interactions. The contributions of partition and adsorption and the effect of the temperature on the retention of analytes were evaluated on all of the stationary phases.     

Single-element ultrasonic transducer modeling using a hybrid FD–PSTD method

In a recent publication [E. Filoux, S. Callé, D. Certon, M. Lethiecq, F. Levassort, Modeling of piezoelectric transducers with combined pseudospectral and finite-difference methods, J. Acoust. Soc. Am. 123 (6) (2008) 4165–4173], a new finite-difference/pseudospectral time-domain (FD–PSTD) algorithm was presented and used to model the generation of acoustic waves by a piezoelectric resonator and their propagation in the structure and the surrounding water. In this paper, the model has been extended to simulate the two-dimensional behaviour of a complete single-element transducer, composed of the resonator, a backing and a front matching layer. This further version of the model takes into account the mechanical loss in materials, and enables the calculation of electrical impedance, which is a characteristic of high interest to optimize the performance of ultrasonic transducers. The impedance curves of a PZT [URL: http://www.ferroperm-piezo.com (last viewed 04/2008); B. Jaffe, R.S. Roth, S. Marzullo, Piezoelectric properties of lead zirconate-lead titanate solid-solution ceramics, J. Appl. Phys. 25 (1954) 809–810] plate-based high-frequency transducer, with a 50 MHz thickness resonant frequency, were compared to those of a KLM model [R. Krimholtz, D.A. Leedom, G.L. Matthei, New equivalent circuit for elementary piezoelectric transducers, Electron. Lett. 6 (1970) 398–399] in the one-dimensional case. The acoustical properties were also found to be in good agreement with those obtained using the finite element (FE) method of ATILA^® software in two-dimensional configuration.     

H?lder metric regularity of set-valued maps

This paper is devoted to metric regularity of set-valued maps from a complete metric space to a Banach space. In particular we extend a known characterization of the regularity modulus to maps defined on reflexive spaces. The higher order metric regularity, i.e. an extension of metric regularity to H?lder context, is also investigated using high order variations of set-valued maps and results of similar nature are obtained for conical metric regularity.     

Space models of degree g+1 of curves of genus g

It is the aim of this note to determine all smooth curves of genus g admitting a birational space model of degree g + 1 whose plane sections define a complete linear series. And we add criteria when there is a smooth such model.