色谱

色谱

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高效液相色谱法测定五味子和含五味子的制剂中五味子乙素及多种活性成分时流动相体系的选择

杨孝容*, 向清祥, 陈稼轩   

  1. Department of Chemistry and Life Science, Leshan Teachers College, Leshan 614004, China
  • 收稿日期:2008-09-17 修回日期:2008-11-17 出版日期:2009-05-30 发布日期:1982-09-25
  • 通讯作者: 杨孝容

Selection of mobile phases for the determination of γ-schisandrin and multi-active constituents in Schisandra chinensis and its preparations by high performance liquid chromatography

YANG Xiaorong*, XIANG Qingxiang, CHEN Jiaxuan   

  1. Department of Chemistry and Life Science, Leshan Teachers College, Leshan 614004, China
  • Received:2008-09-17 Revised:2008-11-17 Online:2009-05-30 Published:1982-09-25
  • Contact: YANG Xiaorong

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719

被引次数

24

摘要： 建立了用高效液相色谱法测定五味子和含五味子的制剂中五味子乙素的流动相体系。用Shim-pack VP-ODS (250 mm×4.6 mm,5 μm)色谱柱,在柱温30 ℃、检测波长285 nm、流速1.0 mL/min的条件下,用不同的流动相组成及其不同比例研究了五味子提取液中3种木脂素(五味子乙素、安五脂素和五味子甲素)的保留时间及其分离情况,从中选择测定五味子乙素的最佳流动相体系。结果表明,在甲醇-水、甲醇-冰醋酸-水的流动相体系中,安五脂素和五味子乙素很难完全分离;而在乙腈-甲醇-水和乙腈-冰醋酸-水流动相体系中,3种木脂素可很好地分离。以乙腈-甲醇-水(体积比为17:58:25)为流动相测定五味子和护肝片中3种木脂素的含量,相对标准偏差(n4)为0.95%～5.8%,平均加标回收率为94.50%～105.6%。将该流动相体系用于供试品中3种木脂素含量的测定,分离效果好,结果令人满意。

关键词: 安五脂素, 高效液相色谱法, 流动相, 五味子, 五味子甲素, 五味子乙素, 中药制剂

Abstract: The systems of mobile phase for the determination of γ-schisandrin in Schisandra chinensis and its preparations were developed by high performance liquid chromatography (HPLC). The separation was performed on a Shim-pack VP-ODS column (250 mm×4.6 mm, 5 μm) at 30 ℃, the detection wavelength was set at 285 nm and the flow rate was 1.0 mL/min. Retention times and separation were investigated in mixed solution of three reference substances (γ-schisandrin, anwulignan, and deoxyschizandrin) and methanol extract of Schisandra chinensis by different systems and proportions of mobile phases to select optimal conditions for the determination of γ-schisandrin. The results showed that the complete separation of γ-schisandrin and anwulignan was difficult in the systems of methanol-water and methanol-acetic acid-water. The separation of γ-schisandrin, anwulignan and deoxyschizandrin can be completed in the systems of acetonitrile-methanol-water and acetonitrile-acetic acid-water when their proportions were suitable. The mobile phase of acetonitrile-methanol-water (17:58:25, v/v/v) was selected for the determination of deoxyschizandrin, γ-schisandrin and anwulignan in Schisandra chinensis and Hugan tablets. The determination results of the three substances were satisfactory with the relative standard deviations (n4) ranged from 0.95% to 5.8%, and the average recoveries ranged from 94.50% to 105.6%. The efficiency of separation and the results of determination were satisfactory for the real samples.

Key words: anwulignan, Chinese herbal preparation , deoxyschizandrin, mobile phase, Schisandra chinensis, γ-schisandrin, high performance liquid chromatography (HPLC)