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试验旨在建立饲料中万古霉素的超高效液相色谱—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—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/mL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0.05 mg/kg,定量限为0.1 mg/kg。在不同饲料中添加浓度范围为0.1~100 mg/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。
The aim of the experiment was to establish a method for the determination of vancomycin in feed by detecting the vancomycin in the sample with 0.05mol / L phosphate buffer-acetonitrile (85:15, V / V) The liquid was purified by a strong cation exchange solid phase extraction column and determined by liquid chromatography-tandem mass spectrometry (MALDI-TOF MS) multi-reaction monitoring mode with external standard method. Vancomycin showed good linearity in the range of 25 ~ 1000ng / mL in different feed matrixes. The limit of detection of vancomycin in feed is 0.05 mg / kg and the limit of quantification is 0.1 mg / kg. The average recoveries of different feeds ranged from 0.1 to 100 mg / kg, with the average recovery of 86.7% -117.1%, the intra-assay CV ranging from 1.0% to 17.4% and the intra-assay CV ranging from 2.9% to 10.1% between. The method has the advantages of fast analysis, high sensitivity and good reproducibility. All the technical indexes meet the requirements of relevant laws and regulations at home and abroad and can be used for the determination of vancomycin in feed.