HPLC法测定盐酸二氟沙星粉中二氟沙星的含量

Content Determination of Difloxacin in Difloxacin Hydrochloride Powder by HPLC

建立并验证了高效液相色谱法测定盐酸二氟沙星粉中二氟沙星含量的方法。采用十八烷基硅烷键合硅胶色谱柱(4.6 mm×250 mm,5μm),以磷酸溶液(取磷酸3.0 m L,加水至1000 m L,用三乙胺调节p H至3.0±0.1,加乙腈50 mL)-甲醇(78∶22,V/V)为流动相,流速为1.0 mL/min,柱温为30℃,波长273 nm。试验结果表明二氟沙星在2~100μg/m L范围内线性良好,R^2=0.9999,平均回收率为98.1%(n=9),RSD为1.0%。本文开发的方法与农业部公告1960号收载的紫外分光光度法相比具有更好的专属性,同时简便、快速、准确,适用于产品的质量控制。

A method for determination of difloxacin in difloxacin hydrochloride powder by HPLC was developed and validated.Analysis was performed on a C18 column(4.6 mm×250 mm,5μm)with a mobile phase of phosphorous acid solution(3.0 mL phosphoric acid was diluted to 1000 mL water and adjusted with triethylamine to pH of 3.0±0.1,then add 50 mL acetonitrile)-methanol(78∶22,V/V)with a 1.0 mL/min flow rate in 30℃condition.The determination wave length was 273 nm.The results showed that the calibration curve was linear in the range of 2~100μg/mL(R 2=0.9999),and the average recovery was 98.1%(n=9)with RSD of 1.0%.The method in No.1960 bulletin of the Ministry of Agriculture is a ultraviolet spectrophotometry method.In contrast with the ultraviolet spectrophotometry method,the method developed in this article has higher specificity.This method was convenient,rapid,and accurate,which was suitable to control the quality of difloxacin hydrochloride powder.