RESUMEN
Determination and kinetics of enrofloxacin and ciprofloxacin in Tra catfish (Pangasianodon hypophthalmus) and giant freshwater prawn (Macrobrachium rosenbergii) using a liquid chromatography/mass spectrometry method. J. vet. Pharmacol. Therap. 34, 142-152. The fluoroquinolones enrofloxacin (EF) and ciprofloxacin (CF) residues were investigated in the edible tissues of two important Asian aquacultured species such as Tra catfish (Pangasianodon hypophthalmus) and giant freshwater prawn (Macrobrachium rosenbergii) using a sensitive liquid chromatography-electrospray ionization-tandem mass spectrometry method. Fish and prawn were treated with medicated feed with multiple doses of EF, in field conditions. A validation study of the analytical method was realized in terms of linearity, specificity, precision (repeatability and within-laboratory reproducibility), recovery and decision limit (CCα). The time needed before the antibiotic disappears from animal tissues or reach the maximum residue limit (MRL, 100µg/kg) was assessed. The concentration values of EF detected in Tra catfish tissue were between the MRL and 2×MRL concentrations, according to the fish density, 7days following the end of the enrofloxacin treatment (20mg/kg body weight per day, for seven consecutive days). The concentration value of ER in prawn tissue was lower than the MRL and the limit of quantification (LOQ, 14µg/kg) 5 and 7days after the stop of the EF treatment (50mg/kg body weight per day, for five consecutive days), respectively. The mean detected levels of CF was much lower in comparison with that of EF, indicating that only a small part of EF is metabolized into CF (<5%) in both Tra catfish and prawn.
Asunto(s)
Antiinfecciosos/farmacocinética , Bagres/metabolismo , Ciprofloxacina/farmacocinética , Residuos de Medicamentos/análisis , Fluoroquinolonas/farmacocinética , Palaemonidae/metabolismo , Administración Oral , Alimentación Animal , Animales , Cromatografía Liquida/veterinaria , Ciprofloxacina/análisis , Enrofloxacina , Fluoroquinolonas/análisis , Agua Dulce , Espectrometría de Masas/veterinariaRESUMEN
Beekeepers suspected maize, Zea mays L., treated with imidacloprid to result in substantial loss of honey bee (Hymenoptera: Apidae) colonies in Belgium. The objective of this study was to investigate the potential impact of maize grown from imidacloprid-treated seeds on honey bee mortality. A survey of 16 apiaries was carried out, and all maize fields treated or not with imidacloprid were located within a radius of 3,000 m around the observed apiaries. Samples of honey, beeswax, and bees were collected in three colonies per apiary and analyzed for pesticide contain by liquid chromatography-tandem mass spectrometry and gas chromatography-tandem mass spectrometry. We first found a significant correlation between the number of colonies per apiary and the mortality rates in an apiary. In addition, this mortality rate was inversely correlated with the surface of maize fields treated and not with imidacloprid, suggesting that this pesticide do not interact with bees' fitness. Moreover, a very large number of our samples contained acaricides either prohibited or ineffective against Varroa destructor (Anderson & Trueman) (Acari: Varroidae), suggesting that the treatment methods used by the beekeepers to be inadequate for mite control. Our results support the hypothesis that imidacloprid seed-treated maize has no negative impact on honey bees.
Asunto(s)
Abejas/efectos de los fármacos , Imidazoles/farmacología , Insecticidas/farmacología , Nitrocompuestos/farmacología , Semillas , Zea mays , Animales , Miel/análisis , Imidazoles/química , Insecticidas/química , Neonicotinoides , Nitrocompuestos/química , Residuos de Plaguicidas/química , Ceras/químicaRESUMEN
We report on the development and validation under ISO 17025 criteria of a multi-residue confirmatory method to identify and quantify 17 widely chemically different pesticides (insecticides: Carbofuran, Methiocarb, Pirimicarb, Dimethoate, Fipronil, Imidacloprid; herbicides: Amidosulfuron, Rimsulfuron, Atrazine, Simazine, Chloroturon, Linuron, Isoxaflutole, Metosulam; fungicides: Diethofencarb) and 2 metabolites (Methiocarb sulfoxide and 2-Hydroxytertbutylazine) in honey. This method is based on an on-column liquid-liquid extraction (OCLLE) using diatomaceous earth as inert solid support and liquid chromatography (LC) coupled to mass spectrometry (MS) operating in tandem mode (MS/MS). Method specificity is ensured by checking retention time and theoretical ratio between two transitions from a single precursor ion. Linearity is demonstrated all along the range of concentration that was investigated, from 0.1 to 20 ng g(-1) raw honey, with correlation coefficients ranging from 0.921 to 0.999, depending on chemicals. Recovery rates obtained on home-made quality control samples are between 71 and 90%, well above the range defined by the EC/657/2002 document, but in the range we had fixed to ensure proper quantification, as levels found in real samples could not be corrected for recovery rates. Reproducibility is found to be between 8 and 27%. Calculated CCalpha and CCbeta (0.0002-0.943 ng g(-1) for CCalpha, and 0.0002-1.232 ng g(-1) for CCbeta) show the good sensitivity attained by this multi-residue analytical method. The robustness of the method has been tested in analyzing more than 100 raw honey samples collected from different areas in Belgium, as well as some wax and bee samples, with a slightly adapted procedure.