固相萃取-LC-MS/MS测定鸡蛋中氟喹诺酮类药物残留

Multiresidue determination of fluoroquinolones in eggs by solid-phase extraction-LC-MS/MS

摘要: 目的： 建立同时测定鸡蛋中诺氟沙星、氧氟沙星、培氟沙星、环丙沙星、洛美沙星、达氟沙星、恩诺沙星、沙拉沙星、二氟沙星残留的固相萃取-LC-MS/MS测定方法。 方法： 鸡蛋样品经乙腈沉淀蛋白质和正己烷脱脂后，过HLB固相萃取小柱净化，LC-MS/MS分析，流动相为乙腈-0.1%甲酸(13∶87)，色谱柱为岛津Shim-pack VP-ODS C₁₈柱。 结果： 建立的固相萃取-LC-MS/MS选择性好，灵敏度和准确度均良好。 结论： 建立的方法可作为多种药物残留检测的常规方法。

Abstract: Aim： To establish an analytical method for the simultaneous determination of norfloxacin，ofloxacin，pefloxacin，ciprofloxacin，lomefloxacin，danofloxacin，enrofloxacin，sarafloxacin and difloxacin in eggs using solid-phase extraction-LC-MS/MS. Methods： Egg samples were deproteinized with acetonitrile，followed by defatting with hexane.Then the samples were processed by solid-phase extraction and analyzed by LC-MS/MS using an electrospray source.The separation was carried out on a Shimadzu Shim-pack VP-ODS C₁₈column，with a mobile phase consisting of acetonitrile-0.1% formic acid (13∶87). Results： The validated method was proved to be of high specificity，accuracy and sensitivity. Conclusion： The established method is suitable for the routine residual monitoring of fluoroquinolones.