Tetraciclinas em medicamentos veterinários e produtos lácteos. / Tetraciclinas em medicamentos veterinarios e produtos lacteos.




The objectives of the present study were establish and validate analytical methods (using flow injection analysis - FIA and high performance liquid chromatography - HPLC) for the determination of oxitetracycline (OTC), doxycycline (DC) and tetracycline (TC) in veterinarians drugs and foods (milk and yoghurt). As well as evaluating the stability of these tetracyclines during the thermal processing of milk and during the process of manufacture and storage of the yoghurt. The analyses for FIA were developed based on the emission of fluorescence of the tetracyclines in alkaline solution. The analyses for HPLC were carried through using a stationary phase (C8 of reverse phase), mobile phase [acetate 0.1 mol L-1 + EDTA 25 mmol L-1 + calcium chloride 35 mmol L-1]: methanol (65:35, v/v) and fluorescence detection. In the thermal processing of milk, three distinct procedures of heating were used (microwaves, plate of heating and cooking-stove). The production of the yoghurt was carried through with added milk of tetracyclines, to verify the degradation of antimicrobians during the processing and shelf-life of the product. The parameters evaluated for validation were established for each analyzed matrix (milk and yoghurt). The analyses for FIA showed detectability (120 ng) and the recovery varied of (98 to 104%) for tetracyclines. The results indicated that the FIA method considered is suitable for the determination of tetracyclines in veterinarian formulations. In the chromatographic analyses, the percentage of recovery of the tetracyclines, in the samples of milk and yoghurt was: 108% for OTC, 87% for DC and 99.8% for TC, with limit of quantification of 27; 46 and 33 ng mL-1 for OTC, DC and TC respectively. Higher degradation occurs when the heating was conducted in the heating plate (11; 28 and 15%) for OTC, DC and TC, respectively. It was verified that in the processing of the yoghurt, contaminations with tetracyclines, above of the LMR, that it was not enough to inhibit the fermentative process, and to the end of 30 days of storage (under refrigeration) of the yoghurt, the tetracyclines levels were reduced in 52%, 61% and 67%, for OTC, DC and TC, respectively. The method developed for riboflavin analysis, presented a satisfactory recovery (92%) and limits of detection and quantification (0.22 ug mL-1 and 0.75 ug mL-1, respectively), showing robustness in the presence of fluorescent substances as the tetracyclines.


iogurte tetraciclina chromatography eliminates of high efficiency cromatografia liquida de alta eficiencia tetraciclina analise por injeção de fluxo it analyzes for flow injection leite milk yoghurt

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