分散固相萃取-超高效液相色谱串联质谱法测定 牛肉中7种头孢菌素类药物及其代谢物

Determination of 7 kinds of cephalosporins and its metabolites in beef by dispersion solid-phase extraction with ultra-performance liquid chromato-graphy-tandem mass spectrometry

中文关键词:  头孢菌素类药物  分散固相萃取  超高效液相色谱-串联质谱法  牛肉

英文关键词:cephalosporin drugs  dispersion solid-phase extraction  ultra-performance liquid chromatography- tandem mass spectrometry  beef

中文摘要:

      目的 建立分散固相萃取超高效液相色谱-串联质谱法(dispersion solid-phase extraction with ultra-performance liquid chromatography-tandem mass spectrometry, DSPE-UPLC-MS/MS)同时测定牛肉中7种头孢菌素类药物及其代谢物残留量的方法。方法 样品经乙腈-水溶液提取, C18分散固相萃取净化, 在电喷雾正离子多反应监测模式下进行定量和定性分析。结果 7种头孢菌素类药物及其代谢物的方法检出限和定量限分别为0.4~0.8 μg/kg和1.1~2.3 μg/kg。在3个添加浓度水平的平均回收率为68.3%~95.7%, 相对标准偏差为1.9%~12.5%。结论 该方法快速、准确、灵敏、稳定, 能够满足牛肉中头孢菌素类药物残留的检测。

英文摘要:

      Objective To establish a method for the detection of 7 kinds of cephalosporins and its metabolites in beef by dispersion solid-phase extraction with ultra-performance liquid chromatography-tandem mass spectrometry (DSPE-UPLC-MS/MS). Methods The samples were extracted with acetonitrile and water solution, cleaned up by C18 dispersion solid-phase extraction, and then analyzed in the positive electrospray ionization and recorded with multiple reaction monitoring mode. Results The LODs and LOQs of 7 kinds of cephalosporins and its metabolites were 0.4~0.8 μg/kg and 1.1~2.3 μg/kg, respectively. The recoveries ranged from 68.3% to 95.7% and the relative standard deviations from 1.9% to 12.5%, spiked with 3 levels. Conclusion The method is quick, accurate, sensitive, stable and suitable for the determination of cephalosporin residues in beef.