分散固相萃取-液相色谱串联质谱法快速测定牛奶中利福昔明残留量

Rapid determination of rifaximin in milk by dispersive solid phase extraction coupled with liquid chromatography-tandem mass spectrometry

中文关键词:  利福昔明  牛奶  分散固相萃取  液相色谱串联质谱  残留

英文关键词:rifaximin  milk  dispersive solid phase extraction  liquid chromatography-tandem mass spectrometry  residues

中文摘要:

      目的 建立分散固相萃取-液相色谱串联质谱法快速测定牛奶中利福昔明残留的分析方法。方法 牛奶样品用乙腈提取, 提取液采用分散固相萃取(dispersive solid phase extraction, DSPE)净化, 采用超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)在多反应正离子监测模式下进行监测。以离子对m/z 786.3/151.0进行定性分析、m/z 786.3/754.4进行基质校准外标法定量分析。结果 方法的检出限(limit of detection, LOD)和定量限(limit of quantitation, LOQ)分别为0.2 μg/kg和0.6 μg/kg。方法基质标准曲线线性方程为Y=159.27X+8.25, r2=0.9998, 4个浓度水平加标回收率在77.1%~102%之间, 批内相对标准偏差为2.4%~7.1%, 批间相对标准偏差为3.9%~6.2%。结论 方法简便、快速、准确, 可用于牛奶样品中利福昔明的药物残留快速确证检测分析。

英文摘要:

      Objective To establish a rapid method for determination of rifaximin residues in milk by dispersive solid phase extraction (DSPE) coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods The milk sample was extracted with acetonitrile, purified by DSPE method, and determined by LC-MS/MS under multiple reaction monitoring mode. Qualitative analysis was performed on m/z 786.3/151.0, and quantitative analysis was performed on m/z 786.3/754.4 by matrix calibration external standard method. Results The limit of detection and limit of quantitation were 0.2 μg/kg and 0.6 μg/kg, respectively. Under the optimum conditions, the linear equation of matrix standard curve was Y=159.27X+8.25 (r2=0.9998). The recoveries of rifaximin in milk samples were in the range of 77.1%-102% at 4 fortified levels from 1.0 to 90 μg/kg, with the relative standard deviation within batches of 2.4%-7.1%, and the relative standard deviation between batches was 3.9%-6.2%. Conclusion This method is simple, rapid and accurate, which can be used for the practical determination of rifaximin residues in bovine milk.