盐酸二甲双胍口服溶液有关物质的测定

Determination of related substances in oral solution of metformin hydrochloride

目的建立测定盐酸二甲双胍口服溶液中双氰胺等有关物质的方法。方法采用高效液相色谱法。色谱柱为磺酸基阳离子交换键合硅胶柱,流动相330 mmol/L磷酸二氢铵溶液(磷酸调节pH至2.7),流速1.0 ml/min,检测波长218 nm,柱温45℃,进样量10μl。结果双氰胺,盐酸二甲双胍分别在0.03~2.02μg/ml,0.38~10.14μg/ml范围内,各自峰面积与被测样品浓度呈良好线性关系(r=1.0000、0.9999);精密度、稳定性实验RSD%<2%;双氰胺平均回收率为99.39%,RSD=0.97%(n=9)。结论该方法简便快速,灵敏度高,专属性强,可用于盐酸二甲双胍口服溶液有关物质的测定。

Objective To establish an high performance liquid chromatography(HPLC)method for the determination of dicyandiamide and related substances in metformin hydrochloride oral solution.Methods HPLC was performed on a sulfonic acid based cationic ion-exchange column with the mobile phase of 330 mmol/L ammonium dihydrogen phosphate(adjusted pH 2.7 with phosphoric acid)at the flow of 1.0 ml/min. The detection wavelength was set at 218 nm,the column temperature was 45℃ and the injection volume was 10 μl.Results The related substance dicyandiamide and metformin hydrochloride showed a good linearity in the concentration range of 0.03-2.02 μg/ml and 0.38-10.14 μg/ml(r=1.0000 and 0.9999),respectively;the RSD in both the precision and stability tests were less than 2%;the average recovery rate of dicyandiamide was 99.39%(RSD=0.97%,n=9).Conclusion The present method appears to be simple,rapid,sensitive and specific,which might be used for the determination of related substances in metformin hydrochloride oral solution.