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Multiresidue determination of antibiotics in aquaculture fish samples by HPLC–MS/MS
Author(s) -
CháferPericás Consuelo,
Maquieira Ángel,
Puchades Rosa,
Company Begoña,
Miralles Javier,
Moreno Amelia
Publication year - 2010
Publication title -
aquaculture research
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.646
H-Index - 89
eISSN - 1365-2109
pISSN - 1355-557X
DOI - 10.1111/j.1365-2109.2010.02504.x
Subject(s) - chromatography , high performance liquid chromatography , european union , residue (chemistry) , biology , aquaculture , analyte , extraction (chemistry) , calibration curve , fish <actinopterygii> , antibiotics , detection limit , fishery , chemistry , microbiology and biotechnology , biochemistry , business , economic policy
An analytical method based on HPLC with MS/MS detection was developed and optimized in order to determine the most useful antibiotics (sulphonamides and tetracyclines) used in aquaculture. A simple extraction procedure, without any clean‐up step, was evaluated in order to obtain maximum analyte recovery from fish samples ( Sparus aurata ). A mixture of methanol:water 70:30 (v/v)+1 mL EDTA 0.1 M was selected as optimum extractant solution. Because no matrix effects were observed, a standard calibration curve prepared in mobile phase was used for quantification purposes. Antibiotic‐free fish samples were spiked at different concentration levels and analysed by the optimized HPLC method. The average recoveries ( n =6) obtained were satisfactory, ranging from 88% to 110% at 100 μg kg −1 . The proposed methodology provided limits of detection for the tested antibiotics in the 1.2–16 μg kg −1 range, lower than 100 μg kg −1 , the maximum residue level established by the European Union. Finally, commercial fish samples from different origins were analysed in order to confirm the usefulness of the developed methodology.