液相色谱-质谱联用法检测化妆品中添加的喹诺酮类药物

Determination of quinolones in Cosmetics by liquid chromatography-tandem mass spectrometry

建立同时测定化妆品中的喹诺酮类抗生素(依诺沙星、氟罗沙星、氧氟沙星、诺氟沙星、培氟沙星、环丙沙星、恩诺沙星、沙拉沙星、双氟沙星、莫西沙星)的液相色谱-串联质谱法。方法样品以2%甲酸-乙腈(体积比15∶10)溶液超声提取,离心分离,以0.2%甲酸水-乙腈溶液为流动相,LC-MS/MS测定喹诺酮类抗生素的含量。结果该方法的线性范围为1~50μg/g,相关系数>0.998,加标1~40μg/g时,回收率为84.3%~99.2%,RSD为0.5%~8.5%,检出限为0.1~0.2μg/kg。结论该方法灵敏、快速、准确,适用于化妆品中喹诺酮类抗生素的检测。

To establish an LC-MS/MS method for simultaneous determination of quinolones (enoxacin, fleroxacin, offloxacin, norfloxacin, pefloxacin, ciprofloxacin, enrofloxacin, sarafloxacin, difloxacin and moxifloxacin) in cosmetics.Methods The samples were extracted with acetonitrile -0.2% formic acid (V∶V=15∶10), 0.2% formic acid in water-acetonitrile was used as mobile phase.Quinolones were determined by LC-MS/MS.Results There was a good linear relationship in the range of 1-50 μg/g of quinolones,r>0.998.When added the quinolones standard solution to the cosmetics in the range 1-40 μg/g, the rates of recovery ranged from 84.3 % to 99.2% and the relative standard deviations of this method were 0.5%-8.5%.Conclusion The method is rapid, accurate and applicable to simultaneous determination of quinolones in cosmetics.