A simple, fast, and efficient method was developed for simultaneous determination of 79 pesticides and 13 antibiotics compounds of different chemical classes of pesticides and antibiotics in honey samples by ultra-high performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS). The sample preparation procedure includes homogenization with McIlvaine buffer 0.1 mol L−1 (pH 4), followed by extraction with acetonitrile and cleanup with florisil, using dispersive solid phase extraction (d-SPE). The proposed method was validated with good results, such as linearity (r2 > 0.9901), normality, and independence of the evaluated data, as well as recoveries between 70 and 120 % with relative standard deviation (RSD) <20 % for most of the compounds spiked from 0.1 to 200 μg kg−1. The experimental method limits of detection and quantification were from 0.03 to 1.51 μg kg−1 and from 0.1 to 5 μg kg−1, respectively, for the pesticides. For the antibiotics, the decision limits (0.1 to 2 μg g−1) and the detection capacity (0.12 to 2.81 μg g−1) were below the maximum residue limits (MRLs) established for honey by the Brazilian and European legislation. The method was successfully applied to real samples from different botanical and geographic origins. From them, 44 % presented residues from 0.12 to 10 μg kg−1 of one or more analytes. The proposed method combines the advantages of a quick sample preparation step with the selectivity and sensitivity of the UHPLC-MS/MS and proved to be suitable for routine analyses.
Financed by the National Centre for Research and Development under grant No. SP/I/1/77065/10 by the strategic scientific research and experimental development program:
SYNAT - “Interdisciplinary System for Interactive Scientific and Scientific-Technical Information”.