气相色谱法测定甘草酸二铵原料药中5种有机溶剂残留量

目的:建立同时测定甘草酸二铵原料中5种溶剂(甲醇、乙醇、乙腈、乙酸和N,N-二甲基甲酰胺(DMF))残留量的方法。方法:采用气相色谱法。以DB-624毛细管为色谱柱,氮气为载气,氢火焰离子化检测器,检测器温度240℃,进样口温度200℃,程序升温;以二甲基亚砜为溶剂,采用直接进样方式,测定10批原料药中5种溶剂的残留量。结果:甲醇、乙醇、乙腈、乙酸、DMF检测浓度线性范围分别为7·5～150、12·5～250、1·0～20·5、1·25～25·0、0·21～4·38μg·mL-1(r为0·9992～1·0000);平均回收率(n=9)均在98·0%以上,RSD<8%;10批样品中溶剂残留量均在合格范围内。结论:建立的方法简便、重复性好,能较好地控制甘草酸二铵原料药的质量。

Determination of 5 Residual Organic Solvents in Crude Drug Diammonium Glycyrrhizinate by GC

OBJECTIVE：To develop a method for simultaneous determination of 5 residual solvents（methanol,ethanol,acetonitrile,acetic acid and N,N-dimethylformamide（DMF）） in diammonium glycyrrhizinate.METHODS：GC method was applied.The determination was performed on DB-624 capillary column.Flame ionization detector was used with nitrogen as carrier gas.The detector temperature was 240 ℃ and injector temperature was 200 ℃ through temperature programming.Residual quantities of 5 kinds of solvents in 10 batches of crude drugs were determined by direct sampling using dimethyl sulfoxide as solvent.RESULTS：The linear ranges were 7.5～150 μg·mL-1 for methanol,12.5～250 μg·mL-1 for ethanol,1.0～20.5 μg·mL-1 for acetonitrile,1.25～25.0 μg·mL-1 for acetic acid and 0.21～4.38 μg·mL-1 for DMF（r=0.999 2～1.000 0）.The average recoveries were all more than 98.0%（n=9） with RSD〈8%.Residual solvents were all within reasonable range in 10 batches of samples.CONCLUSION：The method is convenient and reproducible.It is better for quality control of crude drug diammonium glycyrrhizinate.