Multiresidue determination of antibiotics in feed and fish samples for food safety evaluation. Comparison of immunoassay vs LC-MS-MS.

摘要

Antibiotic residues (sulfonamides and tetracyclines) were determined in Gilthead sea bream (Sparus aurata) and feed samples by means of immunoassays and LC-MS-MS (liquid chromatography-mass spectrometry2). A preliminary study to know the withdrawal time of oxytetracycline in Gilthead sea bream samples was also conducted. It was carried out using immunoassays based on photometric detection of horseradish peroxidase (HRP) activity and time-resolved fluorometric detection of coproporphyrin of Platinum (II) (ELISA and TR-FIA, respectively). The results were compared to those obtained using an LC-MS-MS methodology. They showed that approximately 37 days would be the withdrawal time in order not to exceed the MRL and fish could be commercialized with safety. Regarding feed samples analysis, an LC-MS-MS method was optimized including sample treatment. Average recoveries (n = 6) ranging from 78 to 108% were obtained and precision of the method was between 0.2 and 3%. The same sample treatment was applied to the feed immunoanalysis obtaining satisfactory results. Finally, 20 fish and 4 feed samples were analysed in order to confirm the feasibility of the immunoassays for detecting antibiotic residues. Sulfonamide residues were not detected in any fish sample. Tetracycline residues were detected in some fish samples from marine farms, with total concentrations between 2.1 and 152 ng g--1. In all cases, the obtained results correlated well with those achieved by LC-MS-MS. Therefore, the new methodology allows for food safety of the medicated fish.