GC法测定米诺地尔原料药中3种残留溶剂的含量

Determination of 3 residual solvents in minoxidil by GC

建立气相色谱方法,对米诺地尔原料药中残留的甲醇、二氯甲烷和乙酸乙酯进行测定。Agilent DB-624毛细管气相色谱柱,程序升温,进样口温度200℃,氢火焰离子化检测器(FID),检测器温度240℃,顶空进样,载气为氮气。结果:甲醇、二氯甲烷和乙酸乙酯的检出限分别为0.3、0.5和0.5μg/mL;线性相关系数分别为0.9995、0.9990和0.9988;回收率在98.33%~99.32%之间;RSD均低于3.5%。本方法简单快速、专属性、精密度和准确度和耐用性强,可用于米诺地尔原料药中3种残留溶剂的测定。

To establish method for determination of methanol,dichloromethane and ethyl acetate in Active Pharmaceutical Ingredient(API)of Minoxidil.Gas chromatography was performed on Agilent DB-624 capillary column with inlet temperature of 200℃,detection temperature of 240℃ using nitrogen as carrier gas with headspace injection.The limits of detection of methanol,dichloromethane and ethyl acetate were 0.3,0.5 and 0.5μg/mL.The correlation coefficients of linear ranges were 0.9995,0.9990 and 0.9988,respectively.The recoveries were between 98.33% and 99.32%.RSDs of precision tests were all lower than 3.5%.The method is simple,specific,accurate,precise and robust which can be used for determination of 3 residual solvents in API of Minoxidil.