Quinolones and tetracyclines in aquaculture fish by a simple and rapid LC-MS/MS method

Abstract

The determination of antimicrobials in aquaculture fish is important to ensure food safety. Therefore, simple and fast multiresidue methods are needed. A liquid chromatography tandem mass spectrometry method was developed and validated for the quantification of 14 antimicrobials (quinolones and tetracyclines) in fish. Antimicrobials were extracted with trichloroacetic acid and chromatographic separation was achieved with a C18 column and gradient elution (water and acetonitrile). The method was validated (Decision 2002/657/EC) and it was fit for the purpose. Linearities were established in the matrix and the coefficients of determination were ≥0.98. The method was applied to Nile tilapia and rainbow trout (n = 29) and 14% of them contained enrofloxacin at levels above the limit of quantification (12.53-19.01 µg.kg^-1) but below the maximum residue limit (100 µg.kg^-1). Even though prohibited in Brazil and other countries, this antimicrobial reached fish. Measures are needed to ascertain the source of this compound to warrant human safety.

Keywords: Antibiotic; Aquaculture; Chlortetracycline (PubChem CID: 54675777); Ciprofloxacin (PubChem CID: 2764); Confirmatory method; Danofloxacin (PubChem CID: 71335); Difloxacin (PubChem CID: 56206); Doxycycline (PubChem CID: 54671203); Enrofloxacin; Enrofloxacin (PubChem CID: 71188); Fish; Flumequine: (PubChem CID: 3374); Marbofloxacin: (PubChem CID: 60651); Oxytetracycline (PubChem CID: 54675779); Quantification; Tetracycline (PubChem CID: 54675776).