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Purification of Two Triterpenoids from Schisandra chinensis by Macroporous Resin Combined with High-Speed Counter-Current Chromatography

机译:大孔树脂结合高速逆流色谱法纯化五味子中的两种三萜

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摘要

A method for preparative purification of corosolic acid and nigranoic acid from Schisandra chinensis (SC) was established using a combination of macroporous absorption resin column separation and high-speed counter-current chromatography (HSCCC). The crude extracts obtained from SC using 70% ethanol were separated on a macroporous resin column and then eluted with a graded ethanol series. The 70% ethanol fraction was used as the sample for separation of the two triterpenoids by HSCCC. The two-phase solvent system used for HSCCC separation was chloroform–n-butanol– methanol–water (10:0.5:7:4, v/v/v/v). The upper phase was used as the stationary phase of HSCCC. Corosolic acid (16.4 mg) of 96.3% purity and nigranoic acid (9.5 mg) of 98.9% purity were obtained in a one-step HSCCC separation from 100 mg of the sample. The structures of corosolic acid and nigranoic acid were identified by 1Hnuclear magnetic resonance (NMR) and ~(13)C-NMR.
机译:结合大孔吸附树脂柱分离和高速逆流色谱法(HSCCC),建立了五味子中熊果酸和黑芥酸的制备纯化方法。在大孔树脂柱上分离使用70%乙醇从SC中获得的粗提取物,然后用分级乙醇系列洗脱。 70%的乙醇馏分用作通过HSCCC分离两个三萜类化合物的样品。用于HSCCC分离的两相溶剂系统为氯仿-正丁醇-甲醇-水(10:0.5:7:4,v / v / v / v)。上层相用作HSCCC的固定相。从100 mg样品中进行一步HSCCC分离,得到纯度为96.3%的硬脂酸(16.4 mg)和纯度为98.9%的黑芥酸(9.5 mg)。通过1 H核磁共振(NMR)和〜(13)C-NMR鉴定了Corosolic acid和nigranoic acid的结构。

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