Chromatographic determination of oxytetracycline in milk product samples using liquid-liquid microextraction procedure.

Abstract

Miniaturized procedures for chemical analysis give the possibility of a significant reduction in quantities of organic solvents used during isolation and determination processes. Liquid-liquid microextraction (LLME) using butanol as an extractant was investigated to selectively isolate oxytetracycline (OTC) antibiotic residues from dairy products. The optimal conditions of LLME were established after deproteinization of the samples. The isolation procedure for OTC was performed using 700 µL of butanol. The extracts were analysed by HPLC-UV and LC-MS/MS. A satisfactory analyte recovery was achieved in the range 97.6%-98.9%. The concentration of the linearity range of the studied antibiotic should allow its determination at the level of MRL values. The limit of detection during HPLC-UV and LC-MS/MS determination of OTC in milk samples was 9.9·10^-8mol L^-1 (47.85 µg kg^-1) and 5.7·10^-9mol L^-1 (2.75 µg kg^-1), respectively. The precision (1.7%-8.6%) of the methods using LLME isolation of OTC varied depending on the kind of sample and the chromatographic technique used. The developed methods were applied to the analysis of milk and cottage cheese to estimate the presence and detection of OTC content.