Validation of an Analytical Methodology for Determination of Oxytetracycline and Tetracycline Residues in Honey by HPLC with Fluorescence Detection

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Abstract
An analytical method for the determination of OTC and TC residues in honey was developed. Sample treatment involves an extraction in EDTA-McIlvaine buffer, followed by a solid-phase cleanup step. With regard to the cleanup procedure, different SPE cartridges were evaluated and the results presented. The method was validated according to the guidelines laid down by the 2002/657/EC European Decision parameters: decision limit (Ccα) and detection capability (CCβ) were 20 and 21 μg/Kg and 49 and 50 μg/Kg for OTC and TC, respectively, and recoveries of OTC and TC from spiked samples, at three fortification levels, were higher than 87% for both compounds. The analytical method was applied to 57 honey samples. Keywords: Antibiotics; Tetracyclines; Honey; Solid-phase extraction; High-performance liquid chromatography