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高速逆流色谱结合循环模式,用含盐溶剂从川续断中综合分离环烯醚萜苷和三萜皂苷。

Comprehensive separation of iridoid glycosides and triterpenoid saponins from Dipsacus asper with salt-containing solvent by high-speed countercurrent chromatography coupled with recycling mode.

机构信息

Qilu University of Technology (Shandong Academy of Sciences), Shandong Analysis and Test Center, Jinan, P.R. China.

Institute of Traditional Chinese & Ethnic Medicine Resources, Guizhou University of Traditional Chinese Medicine, Guiyang, P.R. China.

出版信息

J Sep Sci. 2020 Apr;43(7):1265-1274. doi: 10.1002/jssc.201901186. Epub 2020 Feb 28.

DOI:10.1002/jssc.201901186
PMID:31961066
Abstract

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.

摘要

作为一种常用的中药,川续断的根用于滋补肝肾、强筋壮骨。然而,从川续断根中综合快速分离主要活性化合物的有效分离策略尚不存在。本研究提供了一种基于 AB-8 大孔树脂柱层析的有效分离方法,采用不同浓度的乙醇-水溶液和两种不同模式的高速逆流色谱法,结合含盐溶剂系统,从川续断根中快速富集和分离。大孔树脂柱层析采用 AB-8 树脂,以乙醇-水溶液的比例为 10、30、40、50 和 80%,作为不同极性的环烯醚萜苷和三萜皂苷的优化富集条件。对于高速逆流色谱分离,将常规模式和循环模式相结合,开发了一种从 30%、40%和 80%乙醇的富集部分分离 12 种化合物(1-12)的策略,包括 6 种高极性环烯醚萜苷(1-6)和 6 种三萜皂苷(7-12)。循环高速逆流色谱分离成功应用于 11 次循环后分离两种异构体(9 和 10)。

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