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

Letícia Rocha Guidi; Flávio Alves Santos; Ana Cláudia S R Ribeiro; Christian Fernandes; Luiza H M Silva; Maria Beatriz A Gloria

doi:10.1016/j.foodchem.2017.11.094

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

Food Chem. 2018 Apr 15:245:1232-1238. doi: 10.1016/j.foodchem.2017.11.094. Epub 2017 Nov 26.

Authors

Letícia Rocha Guidi¹, Flávio Alves Santos², Ana Cláudia S R Ribeiro², Christian Fernandes³, Luiza H M Silva⁴, Maria Beatriz A Gloria⁵

Affiliations

¹ LBqA - Laboratório de Bioquímica de Alimentos, Faculdade de Farmácia, Universidade Federal de Minas Gerais, Av. Antônio Carlos 6627, Belo Horizonte, MG 31270-901, Brazil; LAMEFI - Laboratório de Medidas Físicas, Faculdade de Engenharia de Alimentos, Universidade Federal do Pará, Belém, Pará 66075-900, Brazil.
² LANAGRO - Laboratório Nacional Agropecuário, Ministério da Agricultura, Pecuária e Abastecimento, 33600-000 Pedro Leopoldo, MG, Brazil.
³ LBqA - Laboratório de Bioquímica de Alimentos, Faculdade de Farmácia, Universidade Federal de Minas Gerais, Av. Antônio Carlos 6627, Belo Horizonte, MG 31270-901, Brazil; Laboratório de Controle de Qualidade de Produtos Farmacêuticos e Cosméticos, Faculdade de Farmácia, Universidade Federal de Minas Gerais, Av. Antônio Carlos 6627, Belo Horizonte, MG 31270 901, Brazil.
⁴ LAMEFI - Laboratório de Medidas Físicas, Faculdade de Engenharia de Alimentos, Universidade Federal do Pará, Belém, Pará 66075-900, Brazil.
⁵ LBqA - Laboratório de Bioquímica de Alimentos, Faculdade de Farmácia, Universidade Federal de Minas Gerais, Av. Antônio Carlos 6627, Belo Horizonte, MG 31270-901, Brazil. Electronic address: mbeatriz@ufmg.br.

PMID: 29287347
DOI: 10.1016/j.foodchem.2017.11.094

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).

MeSH terms

Animals
Anti-Bacterial Agents / analysis
Aquaculture / methods
Brazil
Chromatography, Liquid / methods
Cichlids
Enrofloxacin
Fish Products / analysis*
Fluoroquinolones / analysis
Food Analysis / methods
Food Contamination / analysis*
Limit of Detection
Oncorhynchus mykiss
Quinolones / analysis*
Reproducibility of Results
Tandem Mass Spectrometry / methods*
Tetracyclines / analysis*

Substances

Anti-Bacterial Agents
Fluoroquinolones
Quinolones
Tetracyclines
Enrofloxacin