高效液相色谱法测定双氯芬酸钠凝胶的有关物质

Determination of Relative Substances in Diclofenac Sodium Gel by HPLC

建立了双氯芬酸钠凝胶中有关物质的高效液相色谱分离分析方法。采用梯度洗脱的方法对双氯芬酸钠凝胶的有关物质进行分离,流动相A为pH 2.0三氟乙酸溶液-甲醇(80:20),流动相B为乙腈-甲醇(80:20)。采用Waters XBridge色谱柱(5μm,150mm×4.6mm)进行分离,流速为1.0mL/min,进样体积为5μL,二极管阵列检测器,检测波长为254nm,柱温为30℃。在上述色谱条件下,双氯芬酸钠凝胶及特定杂质均在1.0～40.0mg/L质量浓度范围内线性关系良好,相关系数(r)均大于0.99;方法对特定杂质的回收率为97%～104%,相对标准偏差(RSD)不大于3.8%。该法简便、快速、准确、选择性好、灵敏度高,可用于含醇类辅料的双氯芬酸钠凝胶中有关物质的检测。

A high-performance liquid chromatographic（HPLC） method was developed for the determination of relative substances in diclofenac sodium gel.The separation of analyte was performed on a Waters XBridge column（5 μm,150 mm×4.6 mm） at a flow rate of 1.0 mL/min and an injection volume of 5 μL,by a gradient elution using pH 2.0 trifluoroacetic acid-methanol（80：20） as mobile phase A and acetonitrile-methanol（80：20） as mobile phase B.The photo-diode array detector（PDA） was set at 254 nm.The column temperature was 30 ℃.Under the above chromatographic conditions,the calibration curves were linear in the range of 1.0-40.0 mg/L with correlation coefficients more than 0.99.The recoveries for all the specified impurities ranged from 97% to 104% with RSDs not more than 3.8%.The proposed method could be applied in the determination of relative substances in diclofenac sodium gel containing alcohols excipients with the advantages of simplicity,rapidity,accuracy,good selectivity and high sensitivity.