SIMULTANEOUS DETERMINATION OF PESTICIDES AND ANTIBIOTICS RESIDUES IN HONEY SAMPLES BASED ON ULTRA-HIGH PERFORMANCE LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY
D. Orso, L. Floriano, L.C. Ribeiro, N.M.G. Bandeira, O.D. Prestes, R. Zanella
Federal University of Santa Maria, Laboratory of Pesticide Residues Analysis (LARP), Santa Maria - RS, Brazil
A simple, fast and efficient method was developed for simultaneous determination of 79 pesticides and 13 antibiotics of different chemical classes in honey samples by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Sample preparation procedure includes homogenization with McIlvaine buffer 0.1 mol L-1 (pH 4), followed by extraction with acetonitrile and clean-up using dispersive solid phase extraction (d-SPE) with florisil. The proposed method was validated with good results, such as linearity (r2 > 0.9901) and recoveries between 70 and 120% with RSD <20% for most of the compounds spiked from 0.1 to 200 μg kg-1. The experimental method LOD and LOQ for pesticides were from 0.03 to 1.5 μg kg-1 and from 0.1 to 5 μg kg-1, respectively. For the antibiotics, the decision limits (0.1 to 2 μg kg-1) and the detection capacity (0.12 to 2.81 μg kg-1) were below the maximum residues limits established for honey by the Brazilian and by the European legislation. The method was successfully applied to real samples and 44% presented residues from 0.12 to 10 μg kg-1 of one or more analytes. The proposed method is quick, selective and sensitive, being suitable for routine analyses.
Prof. Dr. Renato Zanella
Renato Zanella studied chemistry at the Federal University of Santa Maria (UFSM), Brazil, and received his PhD in chemistry (1994) at the University of Dortmund/Leibniz-Institut für Analytische Wissenschaften (ISAS), Germany. In 1994 he was appointed as Associate Professor of Analytical Chemistry at the UFSM, Brazil. Since 2014 he is a Full Professor at UFSM. His research interests are the development of analytical methods using chromatography coupled to mass spectrometry for the determination of residues and contaminants, like pesticides, endocrine disrupter and veterinary drugs in food and environmental samples, with particular emphasis in the development of new sample preparation strategies. He has published more than 110 papers in international peer-reviewed journals and 10 book chapters in the fields of environmental and analytical chemistry. He was the Director (2006-2008) of the Analytical Chemistry Division from the Brazilian Chemistry Society and since 2013 is the President of the Network for the Analysis of Environmental Quality in Latin America (RACAL), part of the International Association of Environmental Analytical Chemistry (IAEAC).