化妆品中的甲硝唑、氧氟沙星与环丙沙星HPLC检测法

Determination of Metronidazole,Ofloxacin and Ciprofloxacin in Cosmetics by HPLC

目的:建立反相高效液相色谱同时测定化妆品中的甲硝唑、氧氟沙星与环丙沙星方法。方法:以十八烷基硅烷键合硅胶为填充剂,以0.01mol/L四丁基溴化铵溶液(三乙胺调pH至3.0)-甲醇(88:12)为流动相,柱温30℃,流速1.0ml/min。315nm、293nm、277nm分别作为甲硝唑、氧氟沙星、环丙沙星含量测定的检测波长。样品先用乙腈-水(0.1%甲酸)(体积比5:95)溶液提取,经正己烷脱脂后测定。结果:甲硝唑在2.02～50.59μg/ml,氧氟沙星在2.03～50.69μg/ml,环丙沙星在2.02～50.45μg/ml范围内与峰面积线性关系良好,r分别为0.9999,0.9998和0.9999。10,25,40μg/ml三个浓度水平甲硝唑、氧氟沙星和环丙沙星的平均回收率为85.88%～97.20%,RSD为1.11%～6.10%;检测限均为1ng。结论:本法快速、准确、可用于化妆品中擅自添加的甲硝唑、氧氟沙星与环丙沙星的筛查及含量测定。

Objective：A HPLC method was established for the determination of metronidazole,ofloxacin,ciprofloxacin in cosmetics.Methods：The sample was analyzed on C18 column.The mobile phase was 0.01mol/L tetrabutylammonium bromide solution（adjust to pH 3.0 with triethylamine）-methanol（88：12）.Cosmetic sample was extracted with acetonitrile 0.1% formic acid（5：95,by volume）,and degreased by hexane.Results：The calibration curves showed good linearity in the range of 2.02～50.59μg/ml,2.03～ 50.69μg/ml,2.03～50.69μg/ml,2.02～50.45μg/ml for metronidazole,ofloxacin and ciprofloxacin.The recoveries from spiked samples at three concentration levels of 10,25,40μg/ml were ranged from 85.88% to 97.20%,with RSD of 1.11%-6.10%.The detection limit was 1 ng,and the principal components can be well separated.Conclusion：This method is accurate and reproducible,which could be used for scrennning and determination of metronidazole,ofloxacin,ciprofloxacin in cosmetic sample.