Multiresidue determination of antibiotics in aquaculture fish samples by HPLC-MS/MS

Abstract

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 ¢sh samples (Sparus aurata). A mixture of methanol:water 70:30 (v/v)11mL EDTA 0.1M was selected as optimum extractant solution. Because no matrix e¡ects were observed, a standard calibration curve prepared in mobile phase was used for quanti¢cation purposes. Antibiotic-free ¢sh samples were spiked at di¡erent concentration levels and analysed by the optimized HPLC method. The average recoveries (n 5 6) obtained were satisfactory, ranging from 88% to 110% at 100 mg kg À 1 . The proposed methodology provided limits of detection for the tested antibiotics in the 1.2^16 mg kg À 1 range, lower than 100 mg kg À 1 , the maximum residue level established by the European Union. Finally, commercial ¢sh samples from di¡erent origins were analysed in order to con¢rm the usefulness of the developed methodology.

Multiresidue antimicrobial determination in Nile tilapia (Oreochromis Niloticus) cage farming by liquid chromatography tandem mass spectrometry

“…The high antimicrobial concentrations showed in our study and the studies from several countries (Cháfer-Pericás et al, 2010;Samanidou, 2013a,b andMendoza et al, 2012) suggest that further and continuous investigation of antimicrobials residues in fish samples is necessary to ensure no risk to consumers and to prevent possible contamination and the emergence of resistant bacteria. …”

“…Although an adequate withdrawal time is prescribed, in the last decade, concerns have been raised regarding public health issues over the occurrence of antimicrobials through the food chain (Kan and Meijer, 2007). These residues may include the non-altered parent compound and metabolites and/or conjugates (Cháfer-Pericás et al, 2010). Because of the misuse, the antimicrobial residues in products of animal origin brought a concern to consumers.…”

Multiresidue determination of antibiotics in feed and fish samples for food safety evaluation. Comparison of immunoassay vs LC-MS-MS

“…The conditions found for the optimum performance of the ESI interface in the positive mode were: desolvation flow of 600 L h À1 at 300 C, cone flow of 50 L h À1 , source temperature 120 C, and capillary voltage of 3.5 kV. The MRM acquisition conditions of each analyte are described in a previous work (Cháfer-Pericás et al, 2010). Quantification of each antibiotic was carried out with external calibration curves at concentrations between 10 and 1600 ng mL À1 for each analyte.…”

The Analysis of Oxytetracycline Residue in Tissues of Cultured Rainbow Trout (Oncorhynchus Mykiss)

“…Antibiotic residues significantly affect microbiological results and may create false results; thus, if there are some antibiotic residues in consumed fish, this product cannot be considered free of any microbial pollution by relying on microbiologic experiments nor be recommended for use. Therefore, it is necessary to remove antibiotic residues from the consumed residues to confirm results from microbiological findings (28).…”

“…Then, considering the results of the project and the percentage of pollution, a surveying project should be executed and the antibiotic residues be controlled by employing a proper plan and through determination of the required samples throughout the country (19). Despite antibiotic overdosing, accurate healthcare supervision, and control for the relevant regulation about antibiotics in most countries, due to some reasons such as legal gap, ambiguous behavior with law-breakers, treatment with polluted products, absence of professional officials, lack of a national MRL, lack of diagnostic laboratories for veterinary drug residues, and absence of the relevant experts this trend may seriously endanger the health of the users (28,29). The subject of drug residue in aquatic ecosystem with respect to bacterial resistance has been less explored in Iran.…”