色谱

色谱 ›› 2013, Vol. 31 ›› Issue (9): 869-874.DOI: 10.3724/SP.J.1123.2013.03004

• 研究论文 • 上一篇    下一篇

反相高效液相色谱法同时测定甘草酸单铵盐原料药主成分及有关物质含量

赵燕燕1,2, 刘丽艳1, 韩媛媛1, 李月秋1, 王艳2, 石敏健2   

  1. 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, 河北省分析科学技术重点实验室, 河北省化学生物学重点实验室, 河北 保定 071002
  • 收稿日期:2013-03-01 修回日期:2013-04-18 出版日期:2013-09-28 发布日期:2013-09-02
  • 通讯作者: 赵燕燕
  • 基金资助:

    河北省自然科学基金项目(H2013201203);河北省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).

Simultaneous determination of principal components and related substances of raw material drug of ammonium glycyrrhizinate by reversed-phase high performance liquid chromatography

ZHAO Yanyan1,2, LIU Liyan1, HAN Yuanyuan1, LI Yueqiu1, WANG Yan2, SHI Minjian2   

  1. 1. Medical Experimental Center, Hebei University, Baoding 071000, China;
    2. College of Chemistry and Environmental Science, Hebei University; Key Laboratory of Analytical Science and Technology, Hebei Province; Key Laboratory of Chemical Biology, Hebei Province, Baoding 071002, China
  • Received:2013-03-01 Revised:2013-04-18 Online:2013-09-28 Published:2013-09-02

PDF

242

被引次数

5

摘要：

建立了同时测定甘草酸单铵盐原料药中主成分18α-甘草酸、18β-甘草酸及其有关物质A、有关物质B含量的高效液相色谱法,并用于其质量标准的建立。采用Durashell C18色谱柱(250 mm×4.6 mm, 5 μm),以10 mmol/L高氯酸铵(氨水调节pH 8.20)-甲醇(48:52, v/v)为流动相,流速0.80 mL/min,检测波长254 nm,柱温50 ℃,进样量10 μL。在优化的色谱条件下,18α-甘草酸、18β-甘草酸、有关物质A、有关物质B在0.50~100 mg/L范围内线性关系良好(r>0.9999),检出限分别为0.15、0.10、0.10、0.15 mg/L,平均回收率在97.32%~99.33%之间(n=3),相对标准偏差(RSD)在0.05%~1.06%之间。本方法检测灵敏、重现性好,结果准确可靠,可用于甘草酸单铵盐原料药主成分及有关物质的检测分析,有利于其原料药的质量控制。

关键词: 反相高效液相色谱法, 甘草酸单铵盐, 有关物质, 原料药, 主成分

Abstract:

An analytical method for the simultaneous determination of 18α-glycyrrhizic acid, 18β-glycyrrhizinic acid, related substances A and B and drug quality standard by reversed-phase high performance liquid chromatography (RP-HPLC) was established. The assay was carried out on a Durashell-C18 column (250 mm×4.6 mm, 5 μm) with 10 mmol/L ammonium perchlorate (the pH value was adjusted to 8.20 with ammonia)-methanol (48:52, v/v) as mobile phase at a flow rate of 0.80 mL/min, and the detection wavelength was set at 254 nm. The column temperature was 50 ℃ and the injection volume was 10 μL. Under the separation conditions, the calibration curves of the analytes showed good linearities within the mass concentrations of 0.50-100 mg/L (r>0.9999). The detection limits for 18α-glycyrrhizic acid, 18β-glycyrrhizinic acid, related substances A and B were 0.15, 0.10, 0.10, 0.15 mg/L, respectively. The average recoveries were between 97.32% and 99.33% (n=3) with the relative standard deviations (RSDs) between 0.05% and 1.06%. The method is sensitive, reproducible, and the results are accurate and reliable. The method can be used for the determination of principal components and related substances of ammonium glycyrrhizinate for the quality control of raw material drug of ammonium glycyrrhizinate.

Key words: ammonium glycyrrhizinate, principal component, raw material drug, related substances, reversed-phase high performance liquid chromatography (RP-HPLC)

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