Preparative isolation and purification of three rotenoids and one isoflavone from the seeds of Millettia pachycarpa Benth by high-speed counter-current chromatography
Preparative isolation and purification of three rotenoids and one isoflavone from the seeds of Millettia pachycarpa Benth by high-speed counter-current chromatography
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高速逆流色谱法从厚果鸡血藤种子中制备分离纯化三种鱼藤素和一种异黄酮
DOI：
10.1016/j.chroma.2007.11.060
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发表时间：
2008-01-12
影响因子：
4.1
通讯作者：
Wei, Yuquan
中科院分区：
文献类型：
--
作者：
Ye, Haoyu;Chen, Lijuan;Wei, Yuquan
采用分析型和制备型高速逆流色谱法（HSCCC）从中药厚果崖豆藤种子中分离化学活性成分。采用正己烷-乙酸乙酯-甲醇-水（HEMWat：1：0.8：1：0.6，v/v/v/v/v）的两相溶剂体系，采用高速逆流色谱法首次成功地分离纯化了3个类鱼藤素和1个类胡萝卜素。首先在分析型HSCCC上进行分离参数，然后将优化的条件放大到制备型HSCCC。从400 mg的野牡丹种子粗提物中，一次分离得到160.2mg的山毛豆素，14.6mg的4 ′，5 ′-二甲氧基-6，6-二甲基吡喃酮，109.4mg的鱼藤素，6.7mg的6 α，12 α-脱氢鱼藤素，纯度分别为95%、93%、95%、95%。厚果藤采用高效液相色谱法（HPLC）分析化合物的纯度，电喷雾质谱（ESI-MS）、H-1核磁共振（H-1 NMR）和C-13核磁共振（13 C NMR）分析鉴定化合物的结构。这篇论文是一个很好的例子，证明了CCC在分离活性化合物用于新化学实体的临床前试验中所发挥的作用，即使在不同制造商的离心机之间进行放大时也是如此。(c)2007 Elsevier B. V.保留所有权利。
Both analytical and preparative high-speed counter-current chromatography (HSCCC) were used to isolate and separate chemical bioactive constituents from the seeds of Millettia pachycarpa Benth, a famous traditional Chinese medicine. Three rotenoids and one isoflavone were successfully purified for the first time by HSCCC with a two-phase solvent system composed of n-hexane - ethyl acetate-methanol-water (HEMWat) (1:0.8:1:0.6, v/v/v/v). The separation parameters were first performed on the analytical HSCCC and optimized conditions were then scaled up to preparative HSCCC. The separation produced 160.2mg tephrosin, 14.6mg 4',5'-dimethoxy-6,6-dimethylpyranoisoflavone, 109.4mg deguelin, 6.7mg 6a,12a-dehydrodeguelin with respective purities of 95, 93, 95, 95%, in one single run from 400mg crude extract of the seeds of M. pachycarpa Benth. The purity of the isolated compounds was analyzed by high-performance liquid chromatography (HPLC) and their structures were identified by electrospray ionization mass spectrometry (ESI-MS); H-1 nuclear magnetic resonance (H-1 NMR) and C-13 nuclear magnetic resonance (13C NMR) analysis. This paper is an excellent example of the role that CCC is playing in isolating active compounds for pre-clinical trials of new chemical entities, even when scaling up between centrifuges from different manufacturers. (c) 2007 Elsevier B.V. All rights reserved.