HPLC法测定盐酸地芬尼多片中杂质的含量

Determination of Impurity Alkene in Difenidol Hydrochloride Tablets by HPLC

目的:建立HPLC法测定盐酸地芬尼多片中杂质烯化合物含量的方法。方法:采用岛津SHIMADAZU VP-ODS C_(18)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;流速为0.8 ml·min^(-1);检测波长为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,烯化合物的浓度在0.310～6.195μg·ml^(-1)范围内,与峰面积呈良好线性关系,r=0.999 9(n=7);最低检出限为1.24 ng,最低定量限为3.96 ng;低、中、高3种浓度的回收率分别为99.3%(RSD=0.6%)、99.2%(RSD=0.3%)、99.7%(RSD=0.3%)。结论:该方法操作简便、灵敏度高、结果准确,可用于盐酸地芬尼多片有关物质的检查中杂质烯化合物的含量测定。

Objective： To establish an HPLC method for determination of impurity alkene in difenidol hydrochloride tablets. Method： VP-ODS C 18 column （250 mm × 4. 6 mm ,5 um） was used. The mobile phase consisted of 0. 5 % triethylamine solution （adjusted pH to 4.0 with phosphoric acid ） -methanol （44：56） and the flow rate was 0. 8 ml.min-1. The detection wavelength was 210 nm and the column temperature was 30 ℃. Result： Alkene and other impurities were completely separated from difenidol hydrochloride. The linear range of determination was 0. 310-6. 195 ug.ml-1 with the correlation coefficient of 0. 999 9 （n =7）. The LOD was 1.24 ng,and the LOQ was 3.96 ng. The average recovery of low, middle and high concentration was 99. 3% （ RSD = 0. 6% ）, 99. 2% （ RSD = 0. 3 % ） and 99. 7% （RSD = 0. 3% ）, respectively. Conclusion： The method is simple, accurate and sensitive and suitable for determination of impurity alkene in difenidol hydrochloride tablets.