摘要
建立同时测定牛肉中16种氨基糖苷类兽药残留的方法。样品经磷酸盐缓冲液提取,三氯乙酸沉淀蛋白,调节pH值后,HLB固相萃取小柱净化,Hilic Plus色谱柱分离,在电喷雾电离正离子模式下采用超高效液相色谱-串联质谱检测。结果表明,16种氨基糖苷类兽药在25~750μg/kg内线性关系良好,相关系数均大于0.990,检出限为0.006~0.609μg/kg,定量限为0.02~1.83μg/kg。在牛肉中加标回收率为69.09%~115.50%,相对标准偏差为1.04%~16.58%(n=6)。本方法灵敏度、准确度高,适用于牛肉中16种氨基糖苷类兽药的同时测定。
A method was established for simultaneous determination of 16 aminoglycoside(Ag)residues in beef.Samples were extracted with phosphate buffered solution and the proteins were precipitated using trichloroacetic acid.After adjusting the pH,the target compounds were cleaned up on an HLB solid phase extraction(SPE)column,separated on a Hilic Plus column,and detected by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)in the positive ion electrospray ionization mode.The results showed that the calibration curves for the 16 Ags exhibited good linearity in the concentration range of 25–750μg/kg with correlation coefficients greater than 0.990.The limits of detection(LOD)were 0.006–0.609μg/kg and the limits of quantitation(LOQ)were 0.02–1.83μg/kg.The average recoveries at three spiked levels were in the range of 69.09%–115.50%,with relative standard deviations(RSDs)of 1.04%–16.58%(n=6).The method is sensitive,accurate,and suitable for simultaneous determination of the 16 Ags in beef.
作者
刘华文
梁飞燕
辛丽娜
李名路
LIU Huawen;LIANG Feiyan;XIN Lina;LI Minglu(Guangxi-Asean Food Inspection and Testing Center,Nanning 530021,China)
出处
《肉类研究》
北大核心
2024年第8期42-47,共6页
Meat Research
基金
广西壮族自治区市场监督管理局科技计划项目(GXSJKJ2021-3,GXSJKJ2024-15)。
关键词
离子对竞争性结合
牛肉
氨基糖苷类兽药
超高效液相色谱-串联质谱
ion pair competitive binding
beef
aminoglycosides
ultra-high performance liquid chromatography-tandem mass spectrometry
