Comprehensive separation of iridoid glycosides and triterpenoid saponins from Dipsacus asper with salt-containing solvent by high-speed countercurrent chromatography coupled with recycling mode
Comprehensive separation of iridoid glycosides and triterpenoid saponins from Dipsacus asper with salt-containing solvent by high-speed countercurrent chromatography coupled with recycling mode
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DOI：
10.1002/jssc.201901186
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发表时间：
2020-02-28
影响因子：
3.1
通讯作者：
Zhou, Tao
中科院分区：
文献类型：
--
作者：
Yu, Jinqian;Zhang, Jinqiang;Zhou, Tao
川续断根是一种常用的中药材，具有补肝补肾、壮骨壮肌的功效。然而，目前还没有一种有效的分离策略来全面、快速地从杜仲根中分离出主要活性成分。本研究提供了一种基于AB-8大孔树脂柱层析的高效分离方法，采用不同比例的乙醇和两种不同的高速逆流层析方式，结合含盐溶剂体系，快速从杜仲根中富集分离。在AB-8大孔树脂柱上，以10、30、40、50、80%的乙醇为富集剂，对不同极性的环烯醚萜苷和三萜皂苷进行了大孔树脂柱层析。对于高速逆流色谱分离，将常规模式和循环模式相结合，开发了从30%、40%和80%乙醇的浓缩部分中分离出12个化合物(1-12)的策略，其中包括6个高极性环烯醚苷(1-6)和6个三萜皂苷(7-12)。采用循环高速逆流色谱分离技术，在11个循环后成功分离了两个异构体(9和10)。
The roots of Dipsacus asper Wall as a commonly used traditional Chinese medicine are used for tonifying liver and kidney and strengthening bones and muscles. However, an effective separation strategy for comprehensive and rapid separation of the main active compounds from the roots of D. asper is nonexistent. This investigation provided an effective separation method based on AB-8 macroporous resin column chromatography using different ratios of ethanol in water and two different modes of high-speed countercurrent chromatography with salt-containing solvent system for rapid enrichment and separation from the roots of D. asper. The macroporous resin column chromatography was performed on AB-8 resin using ethanol in water ratios of 10, 30, 40, 50, and 80% as the optimized enrichment conditions for iridoid glycosides and triterpenoid saponins with different polarities. For high-speed countercurrent chromatography separation, the conventional and recycling modes were combined together to develop a strategy for 12 compounds (1-12) from the enriched parts of 30, 40, and 80% ethanol, including six high-polarity iridoid glycosides (1-6) using inorganic salt-containing solvent system and six triterpenoid saponins (7-12). Recycling high-speed countercurrent chromatography separation was successfully applied to separate two isomers (9 and 10) after 11 cycles.