ANTIBIOTICS RESIDUES IN HONEY: VALIDATION PROCEDURE HONEY ANALYTICAL METHODS VALIDATION

An uncontrolled used of antibiotics and sulphonamides is responsible for the presence of residues in beehive products and contributes to the problem of food safety. The optimisation of analytical methods for the detection of residues of antibacterial drugs (sulphonamides, SPs; tylosin, TL; streptomycin, ST) in honey was pursued and the methods applied to routine samples. ST was investigated by liquid chromatographic technique with a post column reaction and fluorimetric detection. SPs were quantified by HPLC equipped with fluorimetric detector and C8 column after a precolumn derivatisation by fluorescamine. The presence of TL residues in honey was confirmed by liquid chromatography – tandem mass spectrometric detection. Chromatographic separation of TL was performed on a C18 column. The validation parameters obtained with these methods were: 88%, 101% and 95-102% for recovery and 10 ng/g, 5 ng/g and 1 ng/g as quantification limits for ST, TL and SPs, respectively.