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摘要
An ultra-high performance liquid chromatography-tandem mass spectrometric (UPLC-MS/MS) method for simultaneous determination of thirty different species of 'lean meat agents' (including clonidine, cyproheptadine, and other 28 beta-agonists) residues in swine urine was developed. The parameters of separation conditions of liquid chromatography, MS/MS detection parameters and sample preparation procedure were optimized. After centrifuged at 5000 r/min for 5 min, the swine urine samples were performed directly by MCX column. Then the column was washed with 3 mL of water and 3 mL of methanol, respectively, and then the compounds were eluted with 5% ammonium hydroxide in methanol. The analytes were detected by UPLC-MS/MS after the elution was evaporated to dryness at 45 degrees C under a stream of nitrogen gas. Under the optimum conditions, thirty of analytes could be well separated in less than 5 min. The linear ranges were 0. 1-10 mu g/L for all analytes with the correlation coefficient (r(2)) higher than 0. 992. Limits of detection (LOD) and limits of quantification (LOQ) of this method were less than 0. 1 mu g/L and 0. 3 mu g/L, respectively. The mean recoveries of three spiked concentration levels in blank sample varied from 67. 6% to 103. 2% with the intra. and inter. relative standard deviations of 2. 8% to 16. 8% and 2. 6% to 15. 8%, respectively. Overall, the proposed method is simple, quick, reliable, sensitivity, and can be applied in large scale supervision of illegal usage of 30 kinds of 'lean meat agents'.
- 出版日期2017-1
- 单位安徽农业大学; 中国动物卫生与流行病学中心
