高效液相色谱法测定盐酸地芬尼多原料中杂质烯化合物的含量

Determination of Content of Impurity Alkene in Difenidol Hydrochloride by HPLC

目的建立测定盐酸地芬尼多原料中杂质烯化合物含量的高效液相色谱法。方法采用VP-ODS色谱柱(250 mm×4.6 mm,5μm),以0.5%三乙胺溶液(用磷酸调pH至4.0)-甲醇(44:56)为流动相,流速0.8 mL/min,检测波长210 nm,柱温30℃。结果盐酸地芬尼多与杂质烯化合物及其他杂质完全分离,烯化合物质量浓度在0.3098～6.195μg/mL范围内与峰面积线性关系良好,r=0.9999(n=7);最低检出限为1.24ng,最低定量限为3.96 ng;回收率为99.94%,RSD=0.09%(n=6)。结论所用方法操作简便、灵敏度高、结果准确,可测定盐酸地芬尼多原料及制剂中杂质烯化合物的含量。

Objective To establish an HPLC method for the content determination of impurity alkene in difenidol hydrochloride.Methods The VP-ODS C18 column（250 mm×4.6 mm,5 μm） was adopted.The mobile phase consisted of 0.5%triethylamine solution（adjusted to pH 4.0 with phosphoric acid）-methanol（44 ∶56） and the flow rate was 0.8 mL/min.The detection wavelength was 210 nm and the column temperature was 30 ℃.Results Alkene and other impurities were completely separated from difenidol hydrochloride.The linear range of determination was 0.309 8-6.195 μg/mL with the correlation coefficient of 0.999 9（n=7）;and LOD was 1.24 ng,LOQ was 3.96 ng.The average recovery rate（n=6） was 99.94%（RSD=0.09%）.Conclusion The method is simple,accurate and sensitive,which is suitable for the content determination of impurity alkene in difenidol hydrochloride raw material and its preparations.