| A comprehensive analytical method based on high liquid chromatography-electrospray ionization tandem mass spectrometry(HPLC-ESI-MS/MS) with positive ionization mode with developed for determining 3 Veterinary Medicines. Including, mequindox, carabadox,enrofloxacinin original foods.The chromatographic conditions and mass spectrometry were optimized.The samples were separately extraeted with Cyclohexane-ethyl acetate(v/v=1:1) mixed solution.The water is removed by Anhydrous sodium sulfate,then purified with n-bexane. The peak time(10~17.5min) of the solution were enriched by the GPC and rotary evaporated, then constant volume to 1.5mL.The separation of MEQ,CBX and ENR were carried out on an Hypersil GOLD aQ column(2.1 mm×150 mm,3 μm) using 0.1% formic acid-metuhanol( v/v=3:2) as mobile phases.The target compounds were confirmed and quantified by MS-MS under multiple-reaction monitering(MRM) mode with external standard method.The results showed that the calibration curves of 3 Veterinary Medicines was linear in the range of 10.0-1000.0 μg/L, with correlation coefficients(r) more than 0.99. Recoveries of 3 Veterinary Medicines at spike concentration levels ranged from 70.07% to 85.36% with relative standard deviations were below 11.50%. The detection limits(LOD)were in the range of 0.15~0.3μg/kg and the quantitative limits(LOQ) were 0.5~1.5μg/kg. |
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