Development of an analytical method to detect metabolites of nitrofurans
2013
Douny, Caroline | Widart, Joëlle | De Pauw, Edwin | Silvestre, Frédéric | Kestemont, Patrick | Tu, Huynh Thi | Phuong, Nguyen Thanh | Maghuin-Rogister, Guy | Scippo, Marie-Louise
Nitrofurans, banned antibiotics in the European Union (EU), have often been found in imported aquaculture products in the past and are still found nowadays according to the Rapid Alert System for Feed and Food (RASFF) of the European Commission. A quantitative method based on liquid chromatography coupled to isotopic dilution tandem mass spectrometry (LC–IDMS/MS) was developed for the determination of the residues of four nitrofuran antibiotic residues in shrimps. The experimental protocol consisted of an acid-catalysed release of protein-bound metabolites, followed by derivatisation with 2-nitrobenzaldehyde (NBA). Then, a double liquid–liquid extraction with ethyl acetate was performed before LC–IDMS/MS analysis by positive electrospray ionisation (ES+) with multiple reaction monitoring (MRM) of two transitions per compound. An “in-house” validation of the method for shrimp analysis was conducted according to the EU criteria for the analysis of veterinary drug residues in foods. The decision limits (CCalpha) were 0.08–0.36μgkg−1 and the detection capabilities (CCbeta) were 0.12–0.61μgkg−1, which are both below the minimum required performance limit (MRPL) set at 1μgkg−1 by the EU. The developed method was applied to evaluate the elimination of furazolidone residues in shrimp muscles after a contamination experiment. After 28days of decontamination, a concentration of 115μgkg−1 of furazolidone metabolite 3-amino-2-oxazolidinone (AOZ) was still measured in the shrimp muscle.
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