Resíduos de medicamentos veterinários em músculo bovino: otimização e validação de métodos analíticos qualitativos por cromatografia líquida de ultra eficiência acoplada à espectrometria de massas Q-Orbitrap

Abstract

The presence of residues of veterinary drugs in food can compromise not only public health, but also the participation of a country in the world economy. In this context, two multiclass screening methods in bovine serum muscle tissue were optimized and validated, based on the combination of ultra-performance liquid chromatography and hybrid sequential high-resolution mass spectrometry of the quadrupole-Orbitrap type with heated electrospray ionization in positive and negative modes. In these methods, we adopted a strategy aimed at detecting a wide range of drugs regulated in Brazil, as well as prospecting those antimicrobials not yet monitored, which brings unprecedented advances to food science. Two different sample preparation were evaluated, method A: comprehensive solid-liquid extraction with 0.1% formic acid in an aqueous solution of EDTA 0.1% (w/v)/acetonitrile/methanol (1:1:1, v/v/v), with further extraction assisted by ultrasound; and method B (QueEChERS). In relation to the selectivity, regardless of the methods, the results showed satisfactory results. On the other hand, the detection capability for screening (CCβ), defined as ½ maximum residue limit, above 34% of the analytes showed a rate of false positives results of up to 5% (error β), and the QuEChERS method provided better detection in number of residues (n = 68). Thus, we emphasize that such procedures showed promising potential for application in routine analyses, providing new perspectives in the analysis of residues, in addition to subsidies for a constant direction of the scope of the analytes monitored in this matrix.