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Article Title

A simple multi-residue method for determination of oxytetracycline, tetracycline and chlortetracycline in export buffalo meat by HPLC-photodiode array detector

Abstract

The development of a simple, rapid and sensitive method for residue monitoring of oxytetracycline (OTC), tetracycline (TC) and chlortetracycline (CTC) in buffalo meat samples is described. The principal steps involved extraction in McIIvaine buffer (pH 3.85) followed by a solid phase clean up step. In HPLC, a reversed phase C8 (RP-C8) column was used and compounds were separated at 35°C using a mobile phase of 0.01 M oxalic acid buffer (pH 1.6)/acetonitrile/methanol (77:18:5, v/v/v) at a flow rate of 0.6 mL/min. A wavelength of PDA detector was set at 355 nm. The detection limit of the method was calculated to be 0.031 μg/g and the minimum detectable quantity was found to be 0.062 μg/g. The statistical evaluation demonstrated high absolute recoveries of OTC, TC and CTC from spiked samples at three fortification levels, which were higher than 78% for all drugs. Excellent method repeatability and reproducibility was found by intra- and inter-day assay precision, yielding the coefficients of variation not more than 11.4 and 14.5% at 0.062 μg/g spike concentrations, respectively. The method was also employed for monitoring of 122 export buffalo meat samples collected from different parts of India, in which only 5 samples showed detectable concentration of OTC residues but were lower than the maximum residue limits (MRLs) set by Codex Alimentarius Commission (CAC), European Union (EU), and United States Food and Drug Administration (US-FDA). TC and CTC were absent in all Samples.

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