摘要
试验旨在建立饲料中万古霉素的超高效液相色谱一串联质谱检测方法，以0．05mol／L磷酸盐缓冲液-乙腈（85：15，V／V）提取样品中的万古霉素，提取液经过强阳离子交换固相萃取柱净化，采用液相色谱一串联质谱多反应监测模式进行测定，外标法定量。不同饲料基质中，万古霉素在25～1000ng／mI。浓度范围内呈良好的线性关系。本方法对万古霉素在饲料中的检测限为0．05mg／kg，定量限为0．1mg／kg。在不同饲料中添加浓度范围为0．1～100mg／kg，其平均回收率为86．7％～117．1％，批内变异系数在1．0％～17．4％之间，批间变异系数在2．9％～10．1％之间。本方法分析速度快、灵敏度高、重现性好，各项技术指标均满足国内外相关法规要求，可用于饲料中万古霉素含量的测定。
A method based on ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） had been developed for the determination of vancomyein in feeds. The analyte was extracted with phosphate buffer -aeetonitrile（85 ： 15, V/V）,and cleaned by strong cation exchange solid phase extraction cartridge. Quantification of the analyte was achieved by UPLC-MS/MS with multiple reaction monitoring （MRM） using external standard method. The calibration curves of vaneo- mycin were linear over the concentration ranges of 25 to 1000 ng/mL in different matrix. Detection and quantification limits of the method for the analyte were 0.05 and 0.1 mg/kg in feeds. The average recoveries ranged from 86.7% to 117.1% at the spiked level of 0.1 to 100 mg/kg in feeds. The inter-run and between-run relative standard deviation was 1.0% to 17.4% and 2.9% to 10. 1%,respectively. The method was reliable,sensitive and reproducibility,its performance eould meet the require- ments of the domestic and international legislation. The method adapted to the determination of vancomycin in feeds.
出处
《中国畜牧兽医》
CAS
北大核心
2013年第11期74-78,共5页
China Animal Husbandry & Veterinary Medicine
