Otimização e validação de método de ensaio quantitativo e confirmatório para determinação de multirresíduos de -lactâmicos e tetraciclinas em rim por CLUE-EM/EM

Abstract

This work optimized and validated a test method to determine quantitative and confirmatory multiresidue of â-lactams and tetracyclines in poultry, bovine, equine and swine kidney, using UPLC-MS/M. The validated methodology was based on the extraction, using a mixture water /acetonitrile (8:2), of analytes tissue and extract purification with hexane and phase dispersive BOND ELUT C18. The extract was concentrated to 2 mL at 40°C, filtered through 0.22 ìm membrane and analyzed by UPLC-MS/MS with electrospray ionization source in positive mode. The method has wide linear range of work, being evaluated were selectivity, matrix effect, CCá, CCâ, precision, trueness, LOD, LOQ and robustness. The detection limit was set between 2.5 to 25.0 mg/kg and the quantification limit between 5.0 to 50.0 mg/kg. The method showed repeatability and intermediate reproducibility conditions tested. Trueness was evaluated by the recovery values ranging between 98 and 107%. In assessing the robustness, the changes made in the extraction procedure were relevant level of concentration studied. The measurement uncertainty was estimated taking into account the uncertainty of the calibration curve and intermediate reproducibility of the data.