Determination and survey of tetracyclines residue in honey by high performance liquid chromatography

Oxytetracycline, tetracycline, chlortetracycline and doxycycline in honey were separated by solid phase extraction (SPE) and determined with high performance liquid chromatography (HPLC) with UV/Visible detector. Analysis was carried out using following conditions: XTerra column , mobile phase composed of 0.01M oxalic acid : methanol : acetonitrile (820 : 80 : 100, v/v/v), isocratic pump at a flow rate of 0.9 ml/min. and of injection volume, UV/Visible detector with wavelength of 360nm. The calibration curves of four tetracyclines showed linearity $(\gamma^2>0.999)$ at concentration range of . The recoveries in fortified honey represented more than with low coefficient of variation $( were suspect positive using modified Charm II screening test. Chlortetracycline residue was found in one foreign honey (illegally distributed) tested at concentrations of 0.22 ppm. Conclusively, for more effective control of tetracyclines used in beekeeping should be further survey for residues in honey and also national guidelines (maximum residue limit : MRL) and methods should be obligatory.