超高效液相色谱-串联质谱法同时测定3种水产品中氯霉素、四环素含量

Determination of chloramphenicol and tetracycline in 3 aquatic products by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相-串联质谱法  氯霉素  四环素

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  chloramphenicol  tetracycline

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定3种水产品中氯霉素、四环素的方法。方法 样品经Na2EDTA-Mcllvaine缓冲溶液(pH=4.0±0.5)提取, HLB柱净化, 采用色谱柱Waters Acquity BEH C18柱(50 mm×2.1 mm, 1.7 μm)分离。电离方式为氯霉素使用电喷雾负离子模式; 四环素使用电喷雾正离子模式。检测方式为多反应监测。 结果 该法线性关系良好, 相关系数大于0.999; 平均回收率为80.4%~97.8%; RSD均小于5%。结论 该方法操作简便快速, 准确度高, 可作为水产品中氯霉素、四环素的测定方法。

英文摘要:

      Objective To establish a method for detection of chloramphenicol and tetracycline in 3 kinds of aquatic products by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted by the solution Na2EDTA-Mcllvaine (pH=4.0±0.5), and the extracts were cleaned-up on HLB solid phase extraction column, Waters Acquity BEH C18 column (50 mm×2.1 mm, 1.7 μm) was used to separate chloramphenicol and tetracycline in aquatic products. The ionization method of chloramphenicol was ESI-and the ionization method of tetracycline was ESI+, The detection method was multiple reaction monitoring (MRM). Results There was a good linear relationship with correlation coefficients better than 0.999. the average recoveries were in the range of 80.4%~97.8%, and RSD was less than 5%. Conclusion The method is convenient, quick and accurate, and can be used for the determination of chloramphenicol and tetracycline in aquatic products.