HPLC测定复方盐酸二甲双胍格列苯脲中3种有关物质

目的建立HPLC方法测定复方盐酸二甲双胍格列苯脲片中已知有关物质双氰胺杂质（1）和杂质（2）的含量。方法采用VP-ODS色谱柱,以甲醇-0.03mol.L^-1磷酸二氢铵的0.025%十二烷基磺酸钠溶液（用磷酸调节pH值至3.5±0.05）（67∶33）为流动相,流速为1.0mL.min^-1,柱温为30℃,检测波长双氰胺为215nm,杂质（1）和杂质（2）为300nm。结果双氰胺在0.125~1.25μg.mL^-1范围内具有良好线性关系（r=0.9998）,平均回收率为100.6%（n=9）,RSD=0.8%;杂质（1）和杂质（2）均在0.75~7.50μg.mL^-1范围内具有良好线性关系,平均回收率均为99.9%（n=9）,RSD=0.2%。结论本方法专属性强、操作简便、准确度高、重现性好。

Determination of Three Related Substances in Metformin Hydrochloride and Glibenclamide Tablets by HPLC

Objective To establish a HPLC method for determination of impurity dicyanodiamide and impurity （1） and impurity（2） in Metformin hydrochloride and Glibenclamide Tablets. Methods VP-ODS column was adopted with methanol-water （the water phase was composed of 0. 03mol · L^1 ammonium dihydrogen phosphate and 0. 025% sodium laurylsulfate, which was adjusted pH to 3.5±0. 05 with phosphoric acid）（67 ： 33）as mobile phase. The flow rate was at 1.0mL · min^-1. The detection wavlength were at 215nm and 300nm. The column temperature was 30℃. Results The linear range of dicyanodiamide was 0. 125-1.25μg.mL^-1 （r=0. 9998）. The average recovery rate was 100. 6%（RSD=0. 8%,n=9）. The linear ranges of impurity （1） amd （2） were 0. 75- 7. 50μg.mL^-1. The average recovery rates were 99. 9%（RSD=0.2% ,n=9）. Conclusions The method is simple, accurate and reproducible. It can be used for determination of dicyanodiamide and impurity（1） and impurity（2） in Metformin hydrochloride and Glibenclamide Tablets.