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.
J Sep Sci. 2017 Mar;40(6):1273-1282. doi: 10.1002/jssc.201601066. Epub 2017 Feb 22.
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.
10-去乙酰基巴卡丁 III 是紫杉醇和多西他赛的重要半合成前体，可从红豆杉属植物中提取。本研究采用大孔树脂柱色谱结合高速逆流色谱或反相快速色谱法，从红豆杉属植物的叶和枝部分离和纯化 10-去乙酰基巴卡丁 III（1）、巴卡丁 III（2）和 7β-木糖基-10-去乙酰基紫杉醇（3）。根据高效液相色谱和液质联用定性分析，选择大孔树脂柱色谱分离后，80%甲醇部位。高速逆流色谱分离采用正己烷、乙酸乙酯、甲醇和水（1.6:2.5:1.6:2.5，v/v/v/v）作为溶剂系统，流速为 2.5 mL/min。反相快速色谱分离采用甲醇/水作为流动相，流速为 3 mL/min。高速逆流色谱分离从 100 mg 样品中得到化合物 1（10.2 mg，94.4%）、2（2.1 mg，98.0%）和 3（4.6 mg，98.8%），用时 110 min；反相快速色谱分离从 100 mg 样品中得到化合物 1（9.8 mg，95.6%）和 3（4.9 mg，97.9%），用时 120 min。
