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J Chromatogr A ; 1429: 175-88, 2016 Jan 15.
Artigo em Inglês | MEDLINE | ID: mdl-26726937

RESUMO

A multiclass method for screening and confirmatory analysis of antimicrobial residues in muscle has been developed and validated, according to Commission Decision 2002/657/EC. Sixty-two antibiotics belonging to ten different drug families (amphenicols, beta-lactams, diamino-pyrimidine, lincosamides, macrolides, pleuromutilins, quinolones, rifamycins, sulfonamides and tetracyclines) have been included in the method. After the addition of an aqueous solution of EDTA, the minced muscle was extracted with acetonitrile/water mixture and, later, with pure acetonitrile. The extract was evaporated and redissolved in ammonium acetate buffer prior to LC injection. Instrumental determination was performed by liquid chromatography coupled to hybrid high resolution mass analyser (LC-HRMS/MS) operating in positive electrospray ionization mode. Chromatographic separation was optimized on a Poroshell 120 EC-C18 column (100 × 3.0 mm, 2.7 µm) with gradient using methanol and water containing 0.1% of formic acid as mobile phases. The method was validated in bovine muscle in the range 3.3-150 µg kg(-1) for all antibiotics; for some compounds with MRL higher than 100 µg kg(-1), the validation interval has been extended until 1500 µg kg(-1). The studied performance characteristics were selectivity, linearity, precision, trueness (recovery), decision limits, detection capabilities, detection and quantification limits. Satisfactory quantitative performances were obtained for all the analytes. Ruggedness tests demonstrated the applicability to swine and poultry muscle, too. Finally the wide participation in proficiency tests allowed to investigate in deep the method performances.


Assuntos
Antibacterianos/análise , Análise de Alimentos/métodos , Carne/análise , Animais , Bovinos , Cromatografia Líquida , Resíduos de Drogas/análise , Macrolídeos/análise , Músculos/química , Quinolonas/análise , Sulfonamidas/análise , Suínos , Tetraciclinas/análise , beta-Lactamas/análise
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