色谱

色谱

• 研究论文 • 上一篇    下一篇

高速逆流色谱法分离制备母丁香和公丁香中的5种非挥发性化合物

高璐, 于波*, 杨红   

  1. 辽宁省生物技术与分子药物研发重点实验室, 辽宁师范大学生命科学学院, 辽宁 大连 116029
  • 收稿日期:2011-06-29 修回日期:2011-08-03 出版日期:2011-11-28 发布日期:2011-12-25
  • 通讯作者: 于波,硕士,讲师,研究方向为药物化学. Tel: (0411)85827085
  • 基金资助:

    大连市科技局科技计划项目(2008E11SF162)

Preparative isolation and purification of five non-volatile compounds from Fructus Caryophylli and Flos Caryophylli by high-speed counter-current chromatography

GAO Lu, YU Bo*, YANG Hong   

  1. Liaoning Provincial Key Laboratory of Biotechnology and Drug Discovery, College of Life Science, Liaoning Normal University, Dalian 116029, China
  • Received:2011-06-29 Revised:2011-08-03 Online:2011-11-28 Published:2011-12-25

PDF

490

被引次数

30

摘要： 应用高速逆流色谱法从母丁香和公丁香中快速分离了3种已知非挥发性化合物,并利用相同方法从公丁香中分离出2种色原酮类化合物。两相溶剂系统A为正己烷-乙酸乙酯-甲醇-水(5:8:6:13, v/v/v/v),系统B为正己烷-乙酸乙酯-甲醇-水(5:8:9:10, v/v/v/v),以系统A的上相为固定相,系统A和B的下相为流动相,利用梯度洗脱方式,在主机转速为880 r/min、流速1.2 mL/min条件下,成功地从70 mg母丁香粗提物中分离得到12.3 mg鞣花酸、9.6 mg鼠李素、17.2 mg槲皮素,从50 mg公丁香粗提物中分离得到5,7-二甲氧基-2-甲基色原酮10.2 mg、5,7-二甲氧基-2,6-二甲基色原酮8.6 mg,纯度均在96%以上。各化合物的结构均由质谱和核磁共振氢谱、碳谱鉴定。利用该方法可以对丁香不同药用部位中的非挥发性化合物进行有效的分离和纯化。

关键词: 非挥发性化合物, 高速逆流色谱, 公丁香, 母丁香, 制备

Abstract: A high-speed counter-current chromatographic (HSCCC) method was successfully developed for the isolation of three non-volatile compounds from Fructus Caryophylli and two chromone compounds from Flos Caryophylli. The optimum separation solution systems included system A (n-hexane-ethyl acetate-methanol-water (5:8:6:13, v/v/v/v) and system B (n-hexane-ethyl acetate-methanol-water (5:8:9:10, v/v/v/v). The upper phase of the system A was used as the stationary phase, and the lower phases of the systems A and B as the mobile phases were operated at a flow of 1.2 mL/min, while the apparatus rotated at 880 r/min. The 12.3 mg of ellagic acid, 9.6 mg of rhamnetin, 17.2 mg of quercetin were successfully purified from 70 mg of the crude extract of Fructus Caryophylli by a two-step separation. In the same way, 10.2 mg of 5,7-dimethoxy-2-methylchromone, 8.6 mg of 5,7-dimethoxy-2,6-dimethylchromone were purified from 50 mg of the crude extract of Flos Caryophylli. The purities of the compounds were all over 96% as determined by high performance liquid chromatography (HPLC). The five compounds were indentified by mass spectrometry (MS), 1H-nuclear magnetic resonance (NMR) and 13C-NMR. The results indicate that HSCCC is a powerful technique for the purification of non-volatile compounds from different parts of Eugenia caryophylla Thunb.

Key words: Flos Caryophylli, Fructus Caryophylli, non-volatile compounds, preparation, high-speed counter-current chromatography (HSCCC)