Enrichment and isolation of barbigerone from Millettia pachycarpa Benth. using high-speed counter-current chromatography and preparative HPLC.
Enrichment and isolation of barbigerone from Millettia pachycarpa Benth. using high-speed counter-current chromatography and preparative HPLC.
复制标题
DOI：
10.1002/jssc.200900641
复制
发表时间：
2010-04
影响因子：
3.1
通讯作者：
Haoyu Ye;Shijie Zhong;Yanfang Li;Ming-hai Tang;A. Peng;Jia Hu;Jie Shi;Shicao He;Wenshuang Wu;Li-juan Chen
中科院分区：
文献类型：
--
作者：
Haoyu Ye;Shijie Zhong;Yanfang Li;Ming-hai Tang;A. Peng;Jia Hu;Jie Shi;Shicao He;Wenshuang Wu;Li-juan Chen
抗肿瘤化合物巴比妥沿着与来自厚果崖豆藤的类鱼藤素衍生物的富集。通过两步高速逆流色谱（HSCCC）分离过程进行。在第一步中，从400 mg M的乙酸乙酯提取物中获得155.8 mg目标级分（Fra 6）。厚果藤通过HSCCC，使用正己烷-乙酸乙酯-甲醇-水（5：4：5：3，v/v）的溶剂系统，在正相头对尾洗脱下，巴比妥从5.1%增加到13%。重复HSCCC以消除该初始级分6中的主要污染物。以正己烷-甲醇-水（2：2：1，v/v）为溶剂，正相洗脱，分离65 min，得到22.1 mg巴比格罗酮，纯度为87.7%。最后，采用制备型HPLC进一步分离巴比酮和类鱼藤素衍生物。其结构经ESI-MS、（1）H NMR和（13）C NMR确证。
Enrichment of the anti-tumor compound barbigerone along with a rotenoid derivative from Millettia pachycarpa Benth. was performed by a two-step high-speed counter-current chromatography (HSCCC) separation process. In the first step, 155.8 mg of target fraction (Fra6) was obtained from 400 mg ethyl acetate extract of M. pachycarpa Benth. with an increase in barbigerone from 5.1 to 13% via HSCCC using a solvent system of n-hexane-ethyl acetate-methanol-water (5:4:5:3, v/v) under normal phase head to tail elution. HSCCC was repeated to eliminate the major contaminant in this initial fraction 6. After a separation time of 65 min, 22.1 mg barbigerone of 87.7% purity was obtained from Fra6 with the ternary solvent system of n-hexane-methanol-water (2:2:1, v/v) under normal phase elution. Finally, preparative HPLC was employed for the further isolation of barbigerone and the rotenoid derivative. The structures were confirmed by ESI-MS, (1)H NMR and (13)C NMR.