Determination of residues and metabolites of more than 140 pharmacologically active substances in meat by liquid chromatography coupled to high resolution Orbitrap mass spectrometry

This study reports an analytical method for simultaneous identification, screening and quantification of 164 residues and metabolites of pharmacologically active substances belonging to such therapeutic classes as anti-infectious (antibiotics and chemotheurapeutics), anti-inflammatory and antiparasitic agents (against protozoa, endo- and ectoparasites), corticoids and agents acting on the nervous and reproductive systems, substances with hormonal and thyreostatic action, and beta agonists. Different sample preparation procedures were compared and optimised for the detection of selected veterinary drugs in chicken, porcine and bovine meat by ultra-high performance liquid chromatography coupled to high-resolution Orbitrap mass spectrometry. The optimised instrumental method and sample preparation procedures were validated by fortifying blank matrix at four levels (0.5, 1.0, 1.5, and 2 times the maximum residue limit (MRL)), or at concentrations as low as possible for substances without an MRL. The evaluated performance parameters were selectivity, matrix effect, method and instrument limits of quantification, accuracy, and repeatability. A total of 130 selected compounds in chicken meat, 127 compounds in bovine meat and 123 compounds in porcine meat samples could be quantified with accuracy ranging from 70 to 120% and RSDs less than 30%. Finally, the method was successfully used to detect and quantify veterinary drug residues in real samples found to be suspect using the non-selective qualitative test for the detection of inhibitor substances. The results were confirmed using the relevant one-residue confirmatory methods revealing concentrations of residues higher than MRLs established for several samples. (C) 2019 Elsevier B.V. All rights reserved.