Abstract:A rapid method for the determination of vancomycin residues in animal-origin foods by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS-MS) was presented. The sample was extracted with 0.1% formic acid-acetonitrile (90:10, V/V). The extract was degreased with n-hexane and cleaned up by solid phase extraction on an MCX column, concentrated by nitrogen blowing and diluted again with the mobile phase prior to being analyzed by UPLC-MS-MS. The calibration curve of vancomycin had a good linearity with a correlation coefficient higher than 0.999 9 in the concentration range of 2.0 to 100.0 μg/L. The detection limit of this method was 0.3 μg/kg, and the limit of quantification was 1.0 μg/kg. The recoveries of vancomycin in spiked samples ranged from 70.05% to 102.97% at spiked levels of 10.0, 20.0, 50.0 and 100.0 μg/kg, with relative standard deviations ≤ 4.65%. This method overcame the problems of high matrix effect and low sensitivity, thereby ensuring the accuracy and reproducibility of the results. This method was suitable for determination of vancomycin residues in animal-origin foods, especially high-fat animal-origin foods.