engleski

Development of SPE-HPLC/MS method for aquaculture antibiotics determination in fish farms

Antibiotics are widely used in fish farms to control bacterial infectious diseases and limit fish mortality. The use of antibiotics in food production in general and also in aquaculture is one of the major concerns because there is evidence that their use may cause bacterial resistance. The common introduction of drug supplemented feeds and the lack of effluent treatments in fish farms provide opportunities for drugs to enter the environment. Some authors consider that the overprescription and the misuse of antimicrobials are the major cause of bacterial resistance in the aquaculture context and that the systematic treatment of fish farms effluents should be conshidered. This work focuses on the application of SPE-HPLC analysis of aquaculture antibiotics in fish farm. The antibiotics investigated include tetracyclines (tetracycline and oxytetracycline) the most popular antibiotics used in aquaculture due to its preefficacy, low cost and low toxicity. Quinolones (enrofloxacine and ciprofloxacine), dexamethazone, febantel, sulfadiazine and trimethoprim are also analyzed because they are widely used for treating many types of bacterial diseases in fish. The method involves pre-concentration and clean-up by solid-phase extraction (SPE). The pharmaceuticals were extracted from 100 mL water samples (pH=4) with methanol. Final analysis of selected antibiotics was carried out by high-performance liquid chromatography (HPLC) with gradient elution of mobile phase (0.1% formic acid in acetonitrile and 0.1% formic acid in water) on polar embedded C18 column and detected by mass spectrometry (MS) via an electrospray ionization interface (ESI) in positive mode. Method development includes optimization of the extraction parameters, and optimization of the LC separation and ESI/MS conditions. The performance characteristics of the SPE– HPLC/MS method were established by validation procedure. Selectivity, linearity, limits of detection (LOD) and quantification (LOQ), precision and recovery were studied. Results of the validation procedure confirmed that method is suitable for the planed purpose.

antibiotics; fish food; solid-phase extraction; high-performance liquid chromatography

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