Abstract
ABSTRACT A chromatographic procedure was developed for the determination of oxytetracycline (OTC), tetracycline (TC), chlortetracycline (CTC), doxycycline (DC) and minocycline (MINO) in animal feeds. Clear analyte-rich extracts were obtained using a 1 : 1 acetonitrile/water mixture buffered at pH 3. The extracts were injected into a conventional unprotected C18 chromatographic column and eluted with a mobile phase of 0.05 M sodium dodecyl sulfate/5% 1-butanol/0.01 M oxalic acid at pH 3. Good resolution was achieved for the five compounds, whereas OTC and TC coeluted with an optimized aqueous-organic mobile phase of methanol/acetonitrile/0.01 M oxalic acid at pH 3. Mean recoveries from spiked feed samples were 79, 83, 86, 87 and 95% for OTC, TC, CTC, DC and MINO, respectively, in the 15–100 µg g−1 concentration range. Limits of detection were in the range 0.1–0.4 µg mL−1. No interference was found from other antibiotics (penicillins G and V, amoxicillin, chloramfenicol, thiamfenicol, erythromycin and trimethoprim), sulfonamides (sulfadiazine, sulfamethazine, sulfamethoxazole, sulfamonomethoxine and sulfathiazole), vitamin D3 and benzoic acid. The micellar system also permitted the resolution of CTC, OTC and TC from their 4-epimers. The methodology was applied to the analysis of animal feeds collected from cattle and pig growing farms.
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