离子对-HPLC法测定盐酸二甲双胍含量及有关物质

Ion Pair HPLC Determination of Metformin Hydrochloride and Its Related Substances

目的:建立离子对-HPLC法测定盐酸二甲双胍含量及有关物质的方法。方法:采用Inertsil C_(18)色谱柱(5μm,4.6mm×150mm);以甲醇-5mmol·L^(-1)磷酸二氢钾溶液(含有10mmol·L^(-1)十二烷基磺酸钠,用磷酸调节pH至3.5±0.05),(64:36)为流动相;流速1.0mL·min^(-1);紫外检测波长:233nm用于含量测定,218nm用于有关物质检测;柱温:室温。结果:离子对-HPLC法测定盐酸二甲双胍的线性范围为5～500μg·mL^(-1);相关系数r=0.999 9;日内精密度RSD=0.82％,日间精密度RSD=1.9％(n=5);双氰胺的线性范围为0.08～0.80μg·mL^(-1);相关系数r=0.9999;日内精密度RSD=0.68％,日间精密度RSD=2.3％(n=5);盐酸二甲双胍含量测定高、中、低3种浓度的回收率分别为99.24％,99.53％,99.18％;RSD分别为0.15％,0.18％,0.22％。结论:本法简便、快速、准确、专属性好。

Objective: A HPLC method was established for the determination of metformin hydrochloride and its related substances. Method: The separation was performed on an Inertsil C18 column (5 μm, 4.6 mm × 150 mm ) . The mobile phase was composed of methyl alcohol - 10 mmol · L-1 sodium dodecylsufonate in 5 mmol · L-1 phosphate salt solution ( pH 3.5±0.05) (64:36). The flow rate was 1.0 mL ·min-1. The detection was car-ried out with a UV detector at 233 nm and 218 nm respectively. Column temperature was room temperature. Re-sults: The calibration curve of metformin hydrochloride was linear between 5 - 500 μg · mL-1 ( r = 0. 999 9 ). Intra - day and inter - day RSD were 0. 82% and 1. 9% ( n = 5 ) . The calibration curve of dicyandiamide was linear between 0. 08 - 0. 80 μg ·mL-1 ( r = 0. 999 9 ) . Intra - day and inter - day RSD were 0. 68% and 2. 3% ( n = 5). The quality control Standard was reliable with a recovery rate of 99. 24% , 99. 53% and 99. 18% , RSD of 0. 15% , 0. 18% and 0.22% for solutions 120, 100, 80 μg ·mL-1 respectively. Conclusion: The method is simple, rapid, accurate and is suitable for the determination of metformin hydrochloride and its related substances.