食品科学

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黄蜀葵花中金丝桃苷及其异构体的分离纯化

李 柰,龙立梅,樊 琛,李小波,曹学丽*   

  1. 北京工商大学食品学院,食品添加剂与配料北京高校工程研究中心,北京 100048
  • 出版日期:2015-02-25 发布日期:2015-02-16
  • 通讯作者: 曹学丽
  • 基金资助:

    北京市自然科学基金重点项目(KZ201410011016)

Separation of Hyperoside and Its Isomers from Abelmoschus manihot (L.) Medicus Flowers

LI Nai, LONG Limei, FAN Chen, LI Xiaobo, CAO Xueli*   

  1. Beijing Higher Institution Engineering Research Center of Food Additives and Ingredients, School of Food and Chemical Engineering,
    Beijing Technology and Business University, Beijing 100048, China
  • Online:2015-02-25 Published:2015-02-16
  • Contact: CAO Xueli

摘要:

应用聚酰胺柱层析法和高效制备液相色谱法研究黄蜀葵花(Abelmoschus manihot(L.) Medicus)中金丝桃苷及其异构体分离制备方法。结果表明:黄蜀葵花粗提物经聚酰胺柱层析分离后,50%乙醇洗脱液中可得到金丝桃苷及其异构体的混合物,将混合物冻干后经高效制备液相色谱分离,高效制备液相柱为Calesil A-120(250 mm×21.2 mm,10 μm),流动相为乙腈-0.2%乙酸(15∶85,V/V),上样量20.0 mg,流速25.0 mL/min,柱温30 ℃,检测波长280 nm,得到纯度分布在99%和97%以上的两种纯物质。经核磁共振及质谱分析,鉴定其分别为金丝桃苷和异槲皮苷,二者互为立体异构体。

关键词: 黄蜀葵花, 聚酰胺柱层析, 高效制备液相色谱, 金丝桃苷, 异槲皮苷

Abstract:

Polyamide chromatography and preparative high performance liquid chromatography (HPLC) were used for
the separation and preparation of two isomers of hyperoside from Abelmoschus manihot (L.) Medicus flowers. The results
indicated that the 50% ethanol eluate contained a mixture of hyperoside and its isomers after polyamide chromatography.
Then the freeze-dried mixture was separated by preparative HPLC on Calesil A-120 column (250 mm × 21.2 mm, 10 μm)
with acetonitrile-0.2% aqueous acetic acid (15:85, V/V) as the mobile phase by injecting 20.0 mg of the sample at a flow rate
of 25.0 mL/min; the column temperature was 30 ℃, and detection wavelength was 280 nm. Two isomers were achieved and
identified by MS, 1H and 13C NMR as hyperoside and isoquercitrin with purities of more than 99% and 97%, respectively,
and both were stereoisomer.

Key words: Abelmoschus manihot (L.) Medicus, polyamide chromatography, preparative high performance liquid chromatography, hyperoside, isoquercitrin

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