Development of Methods Based on Isotopic Dilution in Connection with LC-MS to Evaluate the Presence of Veterinary Drugs and Related Chemicals in Aquaculture Fish

AMÉ, M. V.; WUNDERLIN D.A.; MONFERRÁN, M. V.

Rancagua

Workshop; Second Meeting CRP D52039: Development and Strengthening of Radio-Analytical and Complementary Techniques to Control Residues of Veterinary Drugs and Related Chemicals in Aquaculture Products. IAEA-FAO.; 2016

IAEA- UNITED NATIONS

Theresearch project aims to produce state of the art methods for the analysis ofveterinary drugs, including their metabolites and impurities in feed andaquaculture product. At present, four extraction, clean-up and analyticalmethods based on HPLC-MS (both HRMS and MS/MS) have been developed to accountfor different matrix (water, whole fish and fish tissues), starting from smallamount of samples. Analytical methods include both external standards added toan appropriate matrix (spiked water / spiked fish extracts) and also theaddition of isotopic labelled standards to improve the precision and roughnessof the method. Developed methods have been used to evaluate pharmaceuticals,including some veterinary drugs, in river water, wild fish and laboratoryexposed fish. Screening methods based on HPLC-HRMS (QTOF) afforded reasonablesensitivity for the analysis of pharmaceuticals in water, but more limitedcapacity to evaluate these compounds in whole fish. Quantitative methods, basedon isotopic labelled compounds, modern extraction techniques and HPLC-MS/MS(triple quad), resulted in more sensitive and appropriate methods for theevaluation of 20 pharmaceuticals drugs in fish and fish tissues.               The analysis of 15N in water,shrimp and fish from three lakes having different levels of eutrophicationdemonstrate promissory results to propose the use of δ15N inaquaculture water, shrimp and fish to point out risk associated with thepresence of sewage/ manure, raising questions on the safety of aquacultureproducts grew in such eutrophic areas.               Work plan for next year includesfurther validation of analytical methods applied to veterinary medicines,mainly antibiotics (tetracyclines, flumequine and others), looking to verifythe usefulness of these methods for aquaculture, including the study ofbioaccumulation and biotransformation of these compounds, their metabolites andimpurities in fish.