Journal of Food Safety and Quality

Objective To establish a method for the simultaneous determination of quinolones antibiotics (enrofloxacin, ciprofloxacin, norfloxacin, pefloxacin, ofloxacin, lomefloxacin) and doxycycline residues in prepared dishes by high performance liquid chromatography tandem mass spectrometry. Methods The 84% acetonitrile aqueous solution (1% ice acetic acid) was used as extraction solution, Oasis Prime-HLB solid phase extraction column was used to purify and concentrate, all the eluents were collected, nitrogen-blown to nearly dry, and 1 mL of complex solution 10% methanol aqueous solution (containing 1% ice acetic acid) was added to vortex dissolve, and 0.22 μm microporous filter membrane was taken as supernatant. The Waters ACQUITY UPLC TM BEH C18 column (100 mm×2.1 mm, 1.7 μm) was separated, methanol and 0.1% formic acid aqueous solution were used as mobile phase, ionization mode was spray positive ion mode, and the analysis was performed by high performance liquid chromatography tandem mass spectrometry using multiple reaction detection mode. Results The linear correlation of the 7 kinds of antibiotics was good (r>0.9990). The limits of detection were 0.03–0.24 μg/kg and the limits of quantitatation were 0.09–0.72 μg/kg. The recoveries were 84.5%–114.0% and the relative standard deviations were 1.1%–4.1%. Conclusion The method established in this study is convenient, rapid, accurate and stable, and can be used for quantitative analysis of 6 kinds of quinolone veterinary drug residues and doxycycline residues in prepared dishes.

high performance liquid chromatography-tandem mass spectrometry; prepared dishes; antibiotics; quinolones; doxycycline