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目的从维药苦豆子中提取分离及纯化得到氧化苦参碱,并进行初步鉴定。方法利用乙醇回流提取法和乙醇超声提取法制备氧化苦参碱粗品,利用大孔吸附树脂法分离纯化,并对制备工艺进行优化。结果乙醇回流提取的实验条件为:乙醇浓度60%,料液比(g/mL)1:15,提取时间6 h,侵提温度60℃;乙醇超声提取时,乙醇浓度65%,超声提取频率28 MHz,提取时间20 min。此两种方法的提取效果较好。两种粗品分别经LSA-21吸附大孔树脂进行分离纯化,其条件为:pH值10,用不同浓度(60%、45%和30%)乙醇梯度洗脱,其中30%乙醇的洗脱率最高。结论乙醇回流法和超声提取法是制备氧化苦参碱粗品的可行途径,其中超声提取法具有节能、快速等优点,但出膏率不如乙醇回流提取法。利用LSA-21吸附大孔树脂是分离纯化氧化苦参碱的高效低成本的制备方法,与其他传统柱层析分离法比较具有明显优越性。本研究对实验室快速制备氧化苦参碱纯品提供简便工艺。
OBJECTIVE To extract and purify oxymatrine from Sophora alopecuroides and identify it. Methods The crude oxymatrine was prepared by ethanol reflux extraction and ultrasonic extraction of ethanol. The crude oxymatrine was separated and purified by macroporous adsorption resin and the preparation process was optimized. Results The experimental conditions of ethanol reflux extraction were as follows: the concentration of ethanol was 60%, the ratio of solid to liquid (g / mL) was 1:15, the extraction time was 6 h and the temperature of extraction was 60 ℃. 28 MHz, extraction time 20 min. The extraction of these two methods is better. The two crude products were separated and purified by macroporous resin adsorption by LSA-21 respectively under the conditions of pH 10, gradient elution with different concentrations of ethanol (60%, 45% and 30%), and the elution rate of 30% ethanol highest. Conclusion Ethanol reflux and ultrasonic extraction are feasible ways to prepare oxymatrine crude product. Among them, ultrasonic extraction has the advantages of energy saving and rapidity, but the extraction rate is not as good as ethanol reflux extraction. Adsorption of macroporous resin by LSA-21 is an efficient and low cost method for the separation and purification of oxymatrine. Compared with other traditional column chromatography, it has obvious advantages. This study provides a simple and convenient process for rapid laboratory preparation of oxymatrine pure product.