采用高速逆流色谱法和制备高效液相色谱法从密花豆中富集和分离巴比亚酮。
Enrichment and isolation of barbigerone from Millettia pachycarpa Benth. using high-speed counter-current chromatography and preparative HPLC.
机构信息
State Key Laboratory of Biotherapy, West China Hospital, West China Medical School, Sichuan University, Chengdu, PR China.
出版信息
J Sep Sci. 2010 Apr;33(8):1010-7. doi: 10.1002/jssc.200900641.
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.
从密花美登木（Millettia pachycarpa Benth.）的乙酸乙酯提取物中，通过两步高速逆流色谱（HSCCC）分离过程，对具有抗肿瘤活性的化合物 Barbigerone 及其 Rotenoid 衍生物进行了富集。在第一步中，使用正相首尾洗脱的溶剂系统 n-己烷-乙酸乙酯-甲醇-水（5:4:5:3，v/v），从 400mg 密花美登木乙酸乙酯提取物中获得了 155.8mg 的目标馏分（Fra6），Barbigerone 的含量从 5.1%增加到 13%。通过 HSCCC 重复分离，以去除该初始馏分 6 中的主要杂质。经过 65 分钟的分离时间，从 Fra6 中用正相洗脱的 n-己烷-甲醇-水（2:2:1，v/v）三元溶剂系统获得了 22.1mg 纯度为 87.7%的 Barbigerone。最后，采用制备型高效液相色谱法对 Barbigerone 和 Rotenoid 衍生物进行进一步分离。通过 ESI-MS、（1）H NMR 和（13）C NMR 对结构进行了确认。
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