顶空气相色谱法同时测定甘草酸二铵原料中6种有机溶剂残留量  

Simultaneous Determination of Six Residual Organic Solvents in Diammonium Glycyrrhizinate by Headspace GC

作　　者：张轶华 韩学静 张西如 宋更申 

机构地区：[1]河北省食品药品检验院,石家庄050011

出　　处：《中国药师》2012年第12期1713-1715,共3页China Pharmacist

基　　金：河北省2010年科学技术研究与发展计划项目(编号:10276430)

摘　　要：目的:建立同时测定甘草酸二铵原料中6种残留溶剂[甲醇,乙醇,乙腈,乙酸,N,N--二甲基甲酰胺(DMF)和正己醇]的气相色谱(GC)法。方法:采用DB-624毛细管色谱柱;以氮气为载气,FID检测器,检测器温度240℃,进样口温度200℃,程序升温;以水(每5 ml溶液中加1.0 g无水硫酸钠)为溶剂,采用顶空方式进样,测定6种残留溶剂的残留量。结果:甲醇,乙醇,乙腈,乙酸,DMF和正己醇在各自的浓度范围内均具有良好的线性关系(相关系数r均为0.99以上);平均回收率均在98.0%(n=9)以上。结论:本方法操作简便、成本低廉、结果准确、重复性好,可更好地控制药品质量。Objective：To develop a headspace GC method for the simultaneous determination of methanol,ethanol,acetonitrile, acetic acid,N,N-dimethylformamide（DMF） and hexanol in diammonium glycyrrhizinate.Method：GC was applied in the determination of the six residual organic solvents using water（1.0 g anhydrous sodium sulfate dissolved in 5 ml water） as the solvent.Result：A good linear relationship（r≥0.99） was respectively obtained within the concentration range of methanol,ethanol,acetonitrile,acetic acid,DMF and hexanol.The minimum average recovery of the six residual organic solvents was 98.0%（n =9）.Conclusion：The method is simple,convenient,accurate and reproducible.It can be used in the quality control of diammonium glycyrrhizinate.

关 键 词：顶空气相色谱法 甘草酸二铵 残留溶剂 

分 类 号：R917[医药卫生—药物分析学]