中空纤维分离-高效液相色谱法测定氧氟沙星凝胶剂的含量

目的:建立中空纤维离心超滤前处理方法结合高效液相色谱法测定氧氟沙星凝胶剂的含量。方法:凝胶样品经中空纤维离心超滤技术进行纯化,滤除样品溶液中的高分子辅料后,采用HPLC法测定氧氟沙星凝胶剂的含量。采用C₁₈柱,流动相为甲醇-水(30:70,含0.5%的三乙胺,用磷酸调节pH至4.0),流速1.0 mL·min^-1,柱温为室温,检测波长为293 nm。考察不同溶剂对样品含量测定的影响以及中空纤维膜的非特异性吸附。结果:以1 mL的0.1 mol·L^-1盐酸溶液中和凝胶,然后用水稀释制备样品溶液,采用聚偏氟乙烯中空纤维膜对样品进行超滤处理后,对氧氟沙星不存在非特异性吸附且有效去除了高分子凝胶辅料的干扰。氧氟沙星质量浓度在5.10~51.0 μg·mL^-1范围内呈良好的线性关系(r=0.9998);样品平均回收率为100.4%,RSD不大于1.7%。结论:本法经方法学验证,可用于氧氟沙星凝胶剂的含量测定。

Objective:To establish a sample pretreatment method for the determination of ofloxacin in gel by hollow fiber centrifugal ultrafiltration combined with HPLC.Methods:The gel samples were purified by hollow fiber centrifugal ultrafiltration technique,then determined by HPLC after the macromolecule gel materials were removed.The analysis was carried out on a C₁₈ reversed phase column with the mobile phase of methanol-water (30:70,0.5% triethylamine was added and pH was adjusted to 4.0 with phosphoric acid)at a flow rate of 1.0 mL·min^-1,the column temperature was room temperature,and the UV detection wavelength was 293 nm.The influence of different solvents on the content determination as well as nonspecific adsorption of the hollow fiber was investigated.Results:The sample solution was prepared by 1 mL of 0.1 mol·L^-1 hydrochloric acid,and then diluted with water.The results showed that the polymer gel materials were effectively removed from the sample solutions ultrafiltrated with the PVDF hollow fiber membrane.And there was no nonspecific adsorption to ofloxacin.There was a good linearity within the concentration range of 5.10-51.0 μg·mL^-1(r=0.9998).The average recovery was 100.4%.The precision(RSD)was below 1.7%. Conclusion:The established method is proved by methodology validation that it is applicable for the determination of ofloxacin in ofloxacin gel.