ISSN print edition: 0366-6352 ISSN electronic edition: 1336-9075 Registr. No.: MK SR 9/7 Published monthly

Simultaneous determination of 32 antibiotics in aquaculture products using LC-MS/MS

Ganna Fedorova, Vaclav Nebesky, Tomas Randak, and Roman Grabic

South Bohemian Research Center of Aquaculture and Biodiversity of Hydrocenoses, Faculty of Fisheries and Protection of Waters, University of South Bohemia in Ceske Budejovice, Zatisi 728/II, 389 25, Vodnany, Czech Republic

E-mail: gfedorova@frov.jcu.cz

Abstract: An analytical multiclass, multi-residue method for the determination of antibiotics in aquaculture products was developed and validated. A fast, cheap, and straightforward extraction procedure followed by liquid chromatography-tandem mass spectrometry analysis was proposed. This method covers 32 antibiotics of different classes, which are frequently used in aquaculture. Three different extraction procedures were compared, and the extraction with acetonitrile (0.1 vol. % formic acid) showed the best results. The selected extraction procedure was validated at four different fortification levels (10 μg kg⁻¹, 25 μg kg⁻¹, 50 μg kg⁻¹, and 100 μg kg⁻¹). Recoveries of the tested antibiotics ranged from 70 % to 120 %, with the relative standard deviation (RSD) of triplicates lower than 20 %. The limits of quantification (LOQ) ranged from 0.062 μg kg⁻¹ to 4.6 μg kg⁻¹, allowing for the analysis of trace levels of these antibiotics in aquaculture products. The method was applied to the analysis of selected antibiotics in fish and shrimp meat available in the Czech market.

Keywords: antibiotic residues – aquaculture products – LC-MS/MS detection – validation

Full paper is available at www.springerlink.com.

DOI: 10.2478/s11696-013-0428-3

Chemical Papers 68 (1) 29–36 (2014)