对中国国家药品标准甘草酸单铵盐中有关物质及含量检测方法的改进  

Improvement on determination method of related substances of ammonium glycyrrhizinate in national drug standards of China

作　　者：赵燕燕[1,2] 石敏健[2] 刘丽艳[1] 韩媛媛[1] 李杨[2] 

机构地区：[1]河北大学医学实验中心,河北保定071000 [2]河北大学化学与环境科学学院,河北保定071002

出　　处：《河北大学学报（自然科学版）》2014年第4期372-380,共9页Journal of Hebei University(Natural Science Edition)

基　　金：河北省自然科学基金资助项目(H2013201203);河北大学医学学科专项资金建设资助项目(2014A1003);河北教育厅科学研究计划项目(2009315);河北省卫生厅医学科学研究重点课题计划项目(20090570);河北省中医药管理局科研计划课题(2008072)

摘　　要：针对中国国家药品标准（WS1-XG-2002）中,甘草酸单铵盐含量测定方法分析时间长、效率低、不能实现对甘草酸主成分异构体18α-甘草酸（18α-Gly）和18β-甘草酸（18β-Gly）的有效分离,以及未对有关物质进行准确定量分析和质量控制等问题,改进并建立甘草酸单铵盐原料药及不同剂型制剂中有关物质及含量的检测方法.对色谱条件进行优化,采用Durashell-C18柱（4.6mm×250mm,5μm）,以0.01mol/L高氯酸铵（氨水调节pH至8.20）-甲醇（48∶52,V/V）为流动相,流速0.80mL/min,检测波长254nm,柱温50℃,进样量10μL.18α-Gly,18β-Gly,甘草酸单铵盐杂质A和杂质B在0.5~100.0μg/mL内线性关系良好（r=0.999 9）,检出限分别为0.10,0.10,0.15,0.15μg/mL,平均回收率（n=3）为98.06%~101.61%.与中国国家药品标准（WS1-XG-2002）收载的甘草酸类制剂质量标准比较,本实验建立的方法能够实现对主成分异构体的有效分离,并能真实、准确地检测各有关物质的含量,方法精密度,重现性良好,灵敏度高,结果准确可靠,可用于甘草酸单铵盐原料药及其不同剂型制剂的检测分析及质量控制.The method for determination of related substances in raw material drug of ammonium glycyrrhizinate and different dosage form of glycyrrhizin preparations with long retention time and low efficiency in National Drug Standards of China（WS1-XG-2002）,which could not effectively separate 18α-Gly and 18β-Gly,thus could not truly reflect the contents of 18α-Gly,18β-Gly,impurity A and impurity B in the raw materials and pharmaceutical products.The chromatographic conditions were investigated.The assay was carried out on a Durashell-C18column（4.6mm ×250mm,5μm）with 0.01mol/L ammonium perchlorate（the pH value was adjust to 8.20 with ammonia）-methanol（48∶52,V/V）as mobile phase at a flow rate of 0.8mL/min,and the detection wavelength was set at 254 nm.The column temperature was50℃and the injection volume was 10μL.The calibration curves of 18α-Gly,18β-Gly,impurity A and impurity B of ammonium glycyrrhizinate showed good linearities within the mass concentration of 0.5-100.0μg/mL（r=0.999 9）.The detection limits for 18α-Gly,18β-Gly,impurity A and impurity B were0.10,0.10,0.15 and 0.15μg/mL.The average recoveries（n=3）were between 98.06%and 101.61%.Compared with the method for determination of ammonium glycyrrhizinate in National Drug Standards of China,the method could separate 18α-Gly and 18β-Gly,and could quantitative analysis of related substances accurately and reliable.The method is reproducible and sensitive,the results are accurate and reliable.It is suitable for the determination of related substances.The method can be used for the determination of practical components and related substances of ammonium glycyrrhizinate and different dosage form of glycyrrhizin preparations for the quality control of raw material drug of glycyrrhizinate and different dosage form of glycyrrhizin preparations.

关 键 词：甘草酸单铵盐 原料药与不同剂型制剂 高效液相色谱法 

分 类 号：O657.72[理学—分析化学] R9[理学—化学]