Determinação de resíduos de anabolizantes em músculo, pelo e soro bovino por LC-MS/MS: desenvolvimento analítico e estudos in vivo

Abstract

This work involved the optimization and validation of three multi-residue methods for the analysis of anabolic substances in muscle, hair and bovine serum by LC-MS/MS. The last two matrices were also evaluated by an animal experimentation procedure involving the administration of commercial anabolic formulations in bovine animals. The development of the bovine muscle method comprised a total of 39 analytes belonging to the resorcylic acid lactone, steroid and stilbene classes. The method was applied in this work in the exploratory analysis of 80 bovine muscle samples from the National Plan of Residues and Contaminants Control of Ministry of Agriculture, Livestock and Supply of Brazil and specific meat import programs, where the concentration ranges obtained for the detected anabolic steroids were reported. A total of 25 steroids and steroid esters were validated for bovine hair and 30 for bovine serum. Eight animals underwent treatment with intramuscular injections of commercial formulations containing testosterone propionate and boldenone undecylenate. Hair, serum and urine samples were collected from these animals, and four others were kept without hormonal treatment during the experiment. This latter matrix, traditionally used in anabolic monitoring programs, was compared with the others. The detection of the studied analytes in hair was observed only in hair samples collected near the injection site. The serum matrix was able to detect esterified parental forms for up to 11 days after initiation of treatment. The metabolites of these compounds were detected in serum and urine, where boldenone metabolites presented larger detection windows in serum, which proved to be a matrix suitable for implementation in monitoring programs regarding to anabolic substances.