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 chromatography-tandem mass spectrometry

作　　者：崔凤云[1] 张朝晖[1] 李建辉[1] 黄华 严华[1] 云环[1] 刘鑫[1] 齐鹤鸣 何悦[1] 许翔[1] 

机构地区：[1]北京出入境检验检疫局检验检疫技术中心,北京100026 [2]北京市食品安全监控和风险评估中心,北京100041

出　　处：《食品安全质量检测学报》2016年第2期575-583,共9页Journal of Food Safety and Quality

基　　金：北京市科技计划项目(Z141100002614020);北京国检局科技计划项目(2015BK021)~~

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,C_（18）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0.4~0.8μg/kg和1.1~2.3μg/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。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 C_（18） 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.

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 

分 类 号：O657.63[理学—分析化学] TS251.7[理学—化学]