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Efficient purification of active bufadienolides by a class separation method based on hydrophilic solid-phase extraction and reversed-phase high performance liquid chromatography

晓龙添加于 2016-4-15 18:13 | 1260 次阅读 | 0 个评论

作者
Li X, Liu Y, Shen A, Wang C, Yan J, Zhao W, Liang X
摘要
Traditional Chinese medicines (TCMs) have played a significant role in the process of discovering natural bioactive compounds, especially in anticancer therapeutics. However, the components of TCMs are complex mixtures with wide variation in polarity and content, which leads to inefficiency in the process of active compound discovery from TCMs. In this paper, the popular strategy of utilizing \"pre-fractionated natural product libraries\" has been improved by a new class separation approach to accelerate the process. As an example, the skin of Bufo bufo gargarizans Cantor, a well-known TCM, mainly contains two distinct bufadienolide classes: amino acid-conjugated bufadienolides (AACBs) and free form bufadienolides (AAUBs). We utilized hydrophilic interaction liquid chromatography solid-phase extraction (HILIC-SPE) to resolve the two types of bufadienolides, which co-eluted on C18 columns. By this strategy, twelve bufadienolides of the two types were purified via prep-HPLC from one active fraction, and eight of them were identified by (1)H NMR and (13)C NMR. These results indicated that the class separation method not only overcame the limited orthogonality in a 2D-RPLCxRPLC system but also accelerated the process of active compound discovery.
详细资料
- 关键词: Animals; Bufanolides/chemistry/*isolation & purification; Bufo bufo; Chromatography, Reverse-Phase; Magnetic Resonance Spectroscopy; Medicine, Chinese Traditional; Skin/chemistry; Solid Phase Extraction/*methods; Active bufadienolides; Class separation; Hydrophilic solid-phase extraction; Purification; Toad skin
- 文献种类: Journal Article
- 期刊名称: Journal of Pharmaceutical and Biomedical Analysis
- 期刊缩写: J Pharm Biomed Anal
- 期卷页: 2014年第97卷 54-64页
- 地址: Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China. Electronic address: liangxm@dicp.ac.cn
- ISBN: 0731-7085
学科领域自然科学 » 化学
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