title: 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.
abstract: 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 7β-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.
authors.affiliation: School of Pharmaceutical Sciences, Sun Yat-sen University, Guangzhou, China.|Laboratory for Quality Control of Traditional Chinese Medicine, Guangdong Technology Research Center for Advanced Chinese Medicine, Guangzhou, China.
authors.forename: Junfei
authors.initials: J
authors.lastname: Tao
authors.affiliation: School of Pharmaceutical Sciences, Sun Yat-sen University, Guangzhou, China.|Laboratory for Quality Control of Traditional Chinese Medicine, Guangdong Technology Research Center for Advanced Chinese Medicine, Guangzhou, China.
authors.forename: Rongwei
authors.initials: R
authors.lastname: Yan
authors.affiliation: School of Pharmaceutical Sciences, Sun Yat-sen University, Guangzhou, China.|Laboratory for Quality Control of Traditional Chinese Medicine, Guangdong Technology Research Center for Advanced Chinese Medicine, Guangzhou, China.
authors.forename: Leilei
authors.initials: L
authors.lastname: Zhao
authors.affiliation: School of Pharmaceutical Sciences, Sun Yat-sen University, Guangzhou, China.|Laboratory for Quality Control of Traditional Chinese Medicine, Guangdong Technology Research Center for Advanced Chinese Medicine, Guangzhou, China.
authors.forename: Dongmei
authors.initials: D
authors.lastname: Wang
authors.affiliation: School of Pharmaceutical Sciences, Sun Yat-sen University, Guangzhou, China.|Zhongshan WanYuan New Drug R&D Co., Ltd., Zhongshan, China.
authors.forename: Xinjun
authors.initials: X
authors.lastname: Xu
mesh_terms: D001952:Bridged-Ring Compounds / Q000302:isolation & purification*; D002851:Chromatography, High Pressure Liquid; D003377:Countercurrent Distribution; D010936:Plant Extracts / Q000737:chemistry*; D043823:Taxoids / Q000302:isolation & purification*; D020946:Taxus / Q000737:chemistry*
chemical_list: D001952:Bridged-Ring Compounds; D010936:Plant Extracts; D043823:Taxoids; C080625:taxane
keywords: Taxus wallichiana Zucc; flash chromatography; high-speed countercurrent chromatography; macroporous resin