多壁碳纳米管结合APCI-MS法测定动物源性食品中井冈霉素残留

Residue Analysis of Validamycin in Animal Derived Foods by Multi-walled Carbon Nanotubes Combined with APCI-MS

目的:建立超高效液相色谱-大气压化学电离串联质谱法测定动物源性食品中井冈霉素残留的分析方法。方法:猪肉样品经70%甲醇水提取,乙酸乙酯去脂,滤过型多壁碳纳米管净化小柱净化,经AthenaHILIC色谱柱分离,采用大气压化学电离源(APCI)检测,正离子模式扫描,多反应监测(MRM)模式采集,外标法定量。结果:井冈霉素在2.5~100μg/L浓度范围内线性良好,相关系数(R2)为0.9993,定量限为5.0μg/kg;以猪肉为基质,在10、20、50μg/kg 3个加标浓度下,其回收率范围为91%~103%,变异系数CV(n=6)为5.3%。结论:多壁碳纳米管小柱净化效果良好,该方法简单、快速、灵敏度高,可满足动物源性食品中井冈霉素残留量的检测。

Objective:To establish a method for the determination of validamycin residues in animal-derived food by ultra performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry.Methods:Pork samples were extracted with 70%methanol aqueous solution and degreased by ethyl acetate,purified by filtered multi walled carbon nanotube cartridges,separated by Athena HILIC chromatographic column.Acquired using atmospheric pres⁃sure chemical ionization,the positive ion mode scan and multiple reaction monitoring(MRM)mode,and quantified by ex⁃ternal standard method.Results:The linearity of validamycin was good in the range of 2.5~100μg/L,with correlation coeffi⁃cients(R2)was 0.9993,and the limit of quantification(LOQ)of the method was 5.0μg/kg.The recoveries of validamycin in the pork matrices at 3 spiked concentrations of 10,20,50μg/kg were 91%-103%,and the coefficient of variation(CV)(n=6)was 5.3%.Conclusion:The purification effect of multi-walled carbon nanotube cartridges is good.This method is sim⁃ple,rapid,highly sensitive,and can meet the requirements for the detection of validamycin residues in animal-derived foods.