CRCU

Chemical Research in Chinese Universities ›› 2011, Vol. 27 ›› Issue (3): 392-396.

• Articles • Previous Articles     Next Articles

Isolation and Purification of Unstable Iridoid Glucosides from Traditional Chinese Medicine by Preparative High Performance Liquid Chromatography Coupled with Solid-phase Extraction

LI Cun-man2, XIAO Yuan-sheng1, XUE Xing-ya1, FENG Jia-tao1, ZHANG Xiu-li1* and LIANG Xin-miao1*   

  1. 1. Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, P. R. China;
    2. Hebei Research Centre of Analysis and Testing, Hebei University of Science and Technology, Shijiazhuang 050018, P. R. China
  • Received:2010-06-04 Revised:2010-08-20 Online:2011-05-25 Published:2011-04-29
  • Contact: ZHANG Xiu-li, LIANG Xin-miao E-mail:zhangxiuli@dicp.ac.cn; liangxm@dicp.ac.cn
  • Supported by:

    Supported by the Science and Technology Plan of Liaoning Province, China(No.2006226002) and the Project of the Doctor Fund of Hebei University of Science and Technology, China(No.005121).

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Abstract: An efficient preparative method was successfully developed for isolation and purification of unstable components from medicinal plant extracts, using a combined method of preparative high performance liquid chromatography(HPLC) and solid-phase extraction(SPE). The aim of this study was to obtain an effective method with high preparative efficiency and importantly to avoid the transformation of unstable compounds. The preparative HPLC system was based on an LC/MS controlled four-channel autopurification system. The SPE method was performed with a C18 packing material to trap the target compounds and to remove the acidic additive derived from the mobile phase. Using this method, the unstable iridoid glucosides(IGs) as model compounds were successfully isolated and purified from the extract of Hedyotis diffusa Willd. Six IGs(including one new minor IG) and one nucleotide compound were simultaneously obtained, each with a purity of 91% as determined by HPLC. The structures of the isolated compounds were identified by UPLC/Q-TOF MS, UV, 1D and/or 2D NMR. It was demonstrated that the combination of preparative HPLC with SPE is a versatile tool for preparative purification of unstable compounds from complex natural products.

Key words: Unstable compound, Isolation and purification, Preparative high performance liquid chromatography; , Solid-phase extraction, Iridoid glucoside