THE CONFIRMATION AND QUANTIFICATION OF TETRACYCLINE ANTIBIOTIC RESIDUES IN MILK BY LIQUID CHROMATOGRAPHY TANDEM MASS SPECTROMETRY (LC-MS/MS)

Gjylai Alija, Zehra Hajrullai Musliu, Risto Uzunov, Agim Shabani, Dorentina Bexheti

Abstract

Tetracyclines are broad-spectrum antibiotics, so they are widely used to treat infection diseases in veterinary and human medicine. The inappropriate use of antibiotics can lead to the presence of residues in milk and this can pose a risk to health of humans. Therefore, the European Union has established maximum residue levels (MRLs) for most antibiotics in milk and animal tissues. The aim of this study is validation of LC-MS/MS method for detection of tetracyclin (TC) and oxytetrayclin (OTC) antibiotics in milk. The samples were cleaned on an Oasis HLB solid-phase extraction cartridge. Chromatographic separation was carried out on C18 column (50 x 2.1 mm, 1.7µm) with mobile phase A: 0.1% formic acid in water and mobile phase B: 0.1% formic acid in acetonitrile. Validation of the method was performed according the criteria of Commission Decision 2002/657/EC. In validation procedure were evaluated: linearity, decision limit (CCa), detection capability (CCß), accuracy, precision and reproducibility of the method. The results for optimization of MS/MS method are with agreement with reference’s data. The method demonstrated good linearity on the concentration range from 50.0 to 300.0 µg/L CCa and CCß were below MRLs. The precision and reproducibility were evaluated by RSD, % (relative standard deviation,%). The recovery values were varies from 70-105% with RSD <20%. In conclusion, the LC-MS/MS method was sensitive and suitable for routine analysis for detection of these antibiotics in milk.

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