Simultaneous determination of fluoroquinolones in foods of animal origin by a high performance liquid chromatography and a liquid chromatography tandem mass spectrometry with accelerated solvent extraction.

A confirmatory and quantitative method based on a high performance liquid chromatography UV detector (HPLC-UV) and a liquid chromatography tandem mass spectrometry (LC-MS/MS) with an extraction procedure of accelerated solvent extraction (ASE) has been developed for simultaneous determination of 15 kinds of fluoroquinolones in various animal origin food samples. The sample preparation procedures consist of an extraction step with acetonitrile and a cleaning-up step with Oasis HLB cartridge. Parameters for extraction pressure and temperature, cycle of ASE, clean-up, and analysis procedure have been optimized systematically. The recoveries of FQNs spiked in the tissues as the muscle, liver, kidney of swine, bovine, chicken and fish at a concentration range of 10-800μg/kg were found between 70.6% and 111.1% with relative standard deviations (RSD) less than 15% in HPLC. The LOD and LOQ of the HPLC for the 15 FQNs were 3μg/kg and 10μg/kg, respectively, and those of the LC-MS/MS were 0.3 and 1μg/kg, respectively. These rapid and reliable methods can be used to efficiently separate, characterize and quantify the residues of 15 FQNs (Marbofloxacin, Enoxacin, Fleroxacin, Ofloxacin, Pefloxacin, Lomefloxacin, Danofloxacin, Enrofloxacin, Orbifloxacin, Cinoxacin, Gatifloxacin, Sarafloxacin, Difloxacin, Nalidixic Acid, Flumequine) in food of animal origin.