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目的建立同时测定化妆品中氧氟沙星、环丙沙星、依诺沙星的高效液相色谱二极管阵列法及液质联用确证法。方法样品经超声提取,Luna C18柱分离,用高效液相色谱二级管阵列法检测。液质联用法采用Luna C18柱分离;采用正离子电喷雾模式,氧氟沙星、环丙沙星和依诺沙星[M+H],其主要的特征离子分别为m/z362/318,261,109;332/314,245,134;321/303,234,206。用高效液相色谱DAD法测定阳性样品的含量。结果发现氧氟沙星、环丙沙星及依诺沙星的阳性样品,50批样品两法测定结果一致。在5~150mg.L-1范围内线性良好,相关系数大于0.999;平均加标回收率为97.3%～102.5%,RSD小于2.5%。结论建立的方法准确、可靠。高效液相色谱二级管阵列法可供缺乏质谱的基层检验机构筛查和定量,液质联用法法适合配备质谱的实验室进行确证,方便检验能力的协调。
Objective To establish a simultaneous determination of ofloxacin, ciprofloxacin and enoxacin in cosmetics by high performance liquid chromatography with diode array and LC-MS. Methods Samples were sonicated and separated on a Luna C18 column by high performance liquid chromatography with diode array. LC-MS was performed on a Luna C18 column. The main characteristic ions were m / z 362 / 318,261,109, respectively, using positive ion electrospray ionization mode, ofloxacin, ciprofloxacin and enoxacin [M + 332 / 314,245,134; 321 / 303,234,206. The contents of positive samples were determined by high performance liquid chromatography (DAD). The results found ofloxacin, ciprofloxacin and enoxacin positive samples, 50 batches of two samples of the same results. The linearity was good in the range of 5-150 mg.L-1, the correlation coefficient was greater than 0.999. The average recoveries were 97.3% -102.5% with RSD less than 2.5%. Conclusion The method is accurate and reliable. High performance liquid chromatography (HPLC) diode array method can be used for screening and quantification of grassroots testing institutions lacking mass spectrometry. LC / MS methods are suitable for confirming with mass spectrometry laboratories to facilitate the coordination of testing capabilities.