oasis HLB净化和超高效液相色谱-电喷雾串联质谱检测冻虾中阿维菌素类药物残留

Oasis HLB purification and determination of avermectin residues in frozen shrimp by UPLC-MS/MS

建立采用超高效液相色谱-电喷雾电离串联四极杆质谱(UPLC-MS/MS)同时检测冻虾中阿维茵素、伊维菌素、多拉茵素、爱普利诺菌素残留的方法。试样经乙腈提取、浓缩,经HLB固相萃取小柱净化,超高效液相色谱-电喷雾串联质谱法测定。对流动相、监测离子、校正曲线等进行优化和探讨。实验结果表明,4种分析物在5～100 ng/mL范围内线性关系良好,相关系数均大于0.999。4种分析物在2μg/kg,10μg/kg,20μg/kg加标水平的平均回收率为75.1%～92.5%,相对标准偏差为6.78%～9.89%。四种阿维菌素类药物的检出限均可达到0.5μg/kg。

An ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）method was developed for the determination of Avermectin,Doramectin,Eprinomectin,Ivermectin residues in frozen shrimp.The samples were extracted with acctonitrile,condensed,clcaned up with HLB SPE,then detected by utra high performance liquid chromatography with electrospray ionization tandem mass spectrometry in positive mode.Several UPLC-MS/MS conditions were studied including mobile phase,moditoring ions and calibration curve.The results showed the linear range for 4 avermectins was 5-100ng/ml,with the correlation coefficients all above 0.999.The average recovery for adding 4 acctonitriles to the sample was 75.1%-92.5% at the concentration of 2μg/kg,10μg/kg,20μg/kg and the relative standard deviations were 6.78%-9.89%.The limits of detection for 4 avermectins all attained 0.5μg/kg.