HPLC法测定盐酸地巴唑原料及片剂含量

Content Determination of Dibasol Hydrochloridein Raw Material and Tablets by HPLC

目的:建立HPLC法测定盐酸地巴唑原料及片剂含量,并与高氯酸滴定法进行比较。方法:色谱柱:Kromasil C18(250mm×4.6 mm,5μm);流动相:水-甲醇-冰醋酸-三乙胺(45∶55∶0.5∶0.5);流速:1.0 ml·min^-1;检测波长:220 nm;柱温:30℃;进样量:10μl。结果:盐酸地巴唑的线性范围为4.102~205.100μg·ml^-1(r=0.9999),盐酸地巴唑定量限为0.273μg·ml^-1,原料和片剂的回收率分别为101.2%和99.5%,RSD分别为0.9%和1.3%(n=9)。两种方法测定的原料和片剂含量结果无差异。结论:该方法操作简便,专属性强,结果准确,能有效反应药品质量,与高氯酸滴定法测定结果无明显差异,可作为盐酸地巴唑原料及片剂的含量测定方法。

Objective:To establish an HPLC method for the content determination of diabasol hydrochloride in raw material and tablets and compare with the perchloric acid titration.Methods:The HPLC method was performed on a column of Kromasil C18(250 mm×4.6 mm,5μm).The mobile phase was water-methanol-acetic acid-triethylamine(45∶55∶0.5∶0.5)at a flow rate of 1.0 ml·min^-1.The detection wavelength was 220 nm,the temperature was 30℃and the injection volume was 10μl.Results:There was a good linearity within the range of 4.102-205.100μg·ml^-1 for dibasol hydrochloride(r=0.9999)by HPLC.The limit of detection was0.273μg·ml^-1.The average sample recovery of dibasol hydrochloride raw material and tablets was 101.2%and 99.5%with the RSD of0.9%and 1.3%(n=9),respectively.There was no difference in the content of raw materials and tablets determination by the two method.Conclusion:The method is rapid,accurate and specific.No significant difference from the results of perchloric acid titration.It can be used to determine the content of dibasol hydrochloride in raw material and tablets.