【摘要】 以黄柏粗提物中的生物碱在两相溶剂系统中的分配系数K为依据,对正己烷、石油醚、乙酸乙酯、95%乙醇、甲醇、丙酮、蒸馏水等进行不同的搭配组合,以筛选出最适合HSCCC分离黄柏中小檗碱、黄柏碱、巴马丁和白瓜蒌碱4种生物碱的溶剂体系。结果表明:在检测波长为280 nm,温度为25℃,流速为2.0 mL/min,转速为800 r/min的色谱条件下,以石油醚︰乙酸乙酯︰甲醇︰蒸馏水=5︰1︰2︰4的溶剂体系分离生物碱类物质的效果最佳,从50.70 mg黄柏粗提物中分离得到小檗碱22.10 mg、黄柏碱15.42 mg、巴马丁0.80 mg和白瓜蒌碱0.20 mg,经HPLC分析其纯度分别为98.27%、98.54%、97.55%和96.28%,回收率达到99.86%。更多还原

【Abstract】 Based on the distribution coefficient K of alkaloids in the crude extract of phellodendron in two-phase solvent systems, different combinations of n-hexane, petroleum ether, ethyl acetate, 95% ethanol, methanol, acetone and distilled water were carried out to screen out the solvent systems that were most suitable for HSCCC(high speed countercurrent chromatography) separation of berberine, phellodendrine, palmatine and candicine from phellodendron. The results showed that: Under the chromatographic conditions of detecting wavelength at 280 nm, the temperature at 25 ℃, the flow rate at 2.0 mL/min and the speed at 800 r/min, the best effect was obtained when the solvent system of petroleum ether ∶ ethyl acetate ∶ methanol ∶ water=5 ∶ 1 ∶ 2 ∶ 4 was used to separate alkaloids. 22.10 mg berberine, 15.42 mg phellodendrine, 0.80 mg palmatine and 0.20 mg candicine were isolated from 50.70 mg crude extract of phellodendron, and according to HPLC analysis, the recovery rate reached 99.86% with the purity of 98.27%, 98.54%, 97.55% and 96.28% separately for the four alkaloids.更多还原