4.5 Article

Separation and purification of two taxanes and one xylosyl-containing taxane from Taxus wallichiana Zucc.: A comparison between high-speed countercurrent chromatography and reversed-phase flash chromatography

期刊

JOURNAL OF SEPARATION SCIENCE
卷 40, 期 6, 页码 1273-1282

出版社

WILEY-V C H VERLAG GMBH
DOI: 10.1002/jssc.201601066

关键词

flash chromatography; Taxus wallichiana Zucc.; high-speed countercurrent chromatography; macroporous resin

资金

  1. Industry-University-Research Cooperation Program from Science and Technology Department of Guangdong Province [2013B090600058, 2013B090500100]
  2. Science and Technology Plan Project from Science and Technology Department of Guangzhou City [2014Y2-00216]
  3. Innovative Scientific Research Team Introducing Project of Zhongshan City [2015-224]

向作者/读者索取更多资源

10-Deacetylbaccatin III, an important semisynthetic precursor of paclitaxel and docetaxel, can be extracted from Taxus wallichiana Zucc. A process for the isolation and purification of 10-deacetylbaccatin III (1), baccatin III (2), and 7 beta-xylosyl-10-deacetyltaxol (3) from the leaves and branches of Taxus wallichiana Zucc. via macroporous resin column chromatography combined with high-speed countercurrent chromatography or reversed-phase flash chromatography was developed in this study. After fractionation by macroporous resin column chromatography, 80% methanol fraction was selected based on high-performance liquid chromatography and liquid chromatography with mass spectrometry qualitative analysis. A solvent system composed of n-hexane, ethyl acetate, methanol, and water (1.6:2.5: 1.6: 2.5, v/v/v/v) was used for the high-speed countercurrent chromatography separation at a flow rate of 2.5 mL/min. The reversed-phase flash chromatography separation was performed using methanol/water as the mobile phase at a flow rate of 3 mL/min. The high-speed countercurrent chromatography separation produced compounds 1 (10.2 mg, 94.4%), 2 (2.1 mg, 98.0%), and 3 (4.6 mg, 98.8%) from 100 mg of sample within 110 min, while the reversed-phase flash chromatography separation purified compounds 1 (9.8 mg, 95.6%) and 3 (4.9 mg, 97.9%) from 100 mg of sample within 120 min.

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