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An analytical method for the simultaneous determination of tetracycline (TC), oxtetracycline (OTC), chlortetracycline (CTC) with their 4-epimers, and doxycycline (DC) in animal tissues has been developed and validated. The extraction of the analytes from biological matrice was carried out with a 0.02 M oxalic acid (pH=4.0). The samples were cleaned up by using a solid phase extraction procedure with polymeric cartridges. Chromatographic separation was achieved on a C 18 analytical column using a mobile phase consisting of acetonitrile, methanol and 0.02 M oxalic acid in gradient mode. Detection was carried out by UV detector at λ = 355 nm. The method has been validated according to the Commission Decision 2002/657/EC. The recoveries of the analytes from the spiked samples were 50%-80%. The decision limits (CCα) were from 110 to 125 µg/kg and the detection capabilities (CCß) were from 120 to 155 µg/kg, depending on the analytes. The prepared method was successfully verified in the National Residue Control Programme.
Intensive and massive pig production often contributes to excessive administration of antibacterials in veterinary medicine. The misuse and failures to follow the label directions of antibiotics, as well as withdrawal inadequacy, can lead to their residue occurrence in products of animal origin. The residue of drugs may result in many biological adverse effects and allergic reactions in consumers as well as the spread of drug-resistant bacteria and bacterial resistance acquisition. Consolidation of pig production requires ensuring adequate conditions of the maintenance of animals with high health conditions, consistent with the guidelines for animal welfare. At the same time, the control of antibiotics in animals is an important element providing the high quality of pigs breeding, as well as the protection of consumers. In residue monitoring programs, the primary material for the control of antibiotics presence in pigs are tissue samples, collected from animals at the slaughterhouse. However, post-mortem analysis does not give the opportunity of monitoring the usage of antibiotics on the farm during the breeding of animals. In ante mortem drug analysis blood can be used as a diagnostic biological matrix; however, blood sampling is connected with certain disadvantages for the animals and the staff responsible for material collection. The post-mortem detection and presence of antibiotic residues in pork tissues above MRL values very often lead to the recall and destruction of significant quantities of meat, which may contribute to economic losses. Therefore, a strong need to find and implement new methods for ante-mortem detection of antibiotics in animals exists, which minimize interference in animal welfare. The results of preliminary studies demonstrate that oral fluid seems to be an effective tool for monitoring the reasonable treatment and residue avoidance. It offers a cost-effective approach for the screening of large populations of animals. The method of oral fluid collection with cotton rope usage allows for the rapid sampling of material. In case of positive oral fluid ante-mortem analysis results, the slaughtering of animals can be delayed, which can bring the avoidance of costs connected with the non-compliant pig meat destruction.
Medycyna Weterynaryjna
|
2010
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tom 66
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nr 07
s.453-458,tab.,bibliogr.
In this paper the pharmacological properties of azalides, an improved group of macrolide antibiotics, have been reviewed. Worldwide interest in macrolide antibiotics has led to the development of several semi-synthetic derivatives of 14-membered erythromycin, such as 15-membered azithromycin and tulathromycin, with an additional nitrogen atom in the lacton ring. The newer macrolides, called azalides, have broader antibacterial activity against Gram-positive and Gram-negative pathogens as well as atypical pathogens of the respiratory system. They are characterized by better pharmacokinetic parameters, reduced adverse reactions and an improved drug-interaction profile compared with erythromycin. The application of these groups of antibiotics has some advantages over erythromycin, including longer half-lives and higher tissue concentrations, especially at the site of infection, which makes it possible to administer them once a day in the treatment of respiratory tract infections, in contrast to more frequent dosage required for erythromycin. Azalides are more acid-stable and therefore demonstrate greater oral bioavailability. In addition, these antibiotics have immunomodulatory and anti-inflammatory properties, which can be useful in the treatment of chronic disorders. The pharmacokinetic/pharmacodynamic relations, which are important in predicting clinical efficacy of antibiotics, are also reviewed. To ensure food safety, the European Commission had set Maximum Residue Limits (MRLs) for erythromycin, as well as for tulathromycin. However, azythromycin has not been certified for use in food producing animals, and therefore no MRLs have been established for this azalide.
A liquid chromatography - tandem mass spectrometry (LC-MS/MS) method for the determination of Oxytetracycline (OTC), 4-epi oxytetracycline (4-epi OTC), tetracycline (TC), 4-epi tetracycline (4-epi TC), chlortetracycline (CTC), 4-epi chlortetracycline (4-epi CTC), doxycycline (DC), minocycline (MINO), methacycline (META) and rolitetracycline (ROLI) residues in muscles was developed. The procedure consisted of an oxalic acid extraction followed by protein removal with trichloroacetic acid. Further solid phase clean-up on polymeric (Strata X) reversed phase columns was performed to obtain an extract suitable for LC-MS/MS analysis. The tetracyclines were separated on a C 18 analytical column with mobile phase consisting of 0.01% formic acid in acetonitrile and 0.01% formic acid in water in gradient mode. The method was validated according to the Commission Decision 2002/657/EC. The recoveries of all target compounds were 91.8% - 103.6%. The decision limits were from 109.0 to 119.8 µg/kg and detection capability varied within the range of 122.2 to 137.6 µg/kg, depending on the analyte.
Microbial and biochemical analyses of soil under winter wheat in a field trial with various cultivation systems (organic, conventional and monoculture) were performed during 3 growing seasons: 2001, 2002 and 2003. The activities of the tested enzymes (dehydrogenase and phosphatases) and microbial biomass C and N contents in the monoculture soil were generally significantly lower than those in the soil from the organic and conventional–short rotation systems, indicating that substantial disturbances may occur in the microbial activity of the monoculture soil.
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