从苦豆子中分离纯化苦参碱和槐定碱的工艺研究

运用稀酸水法从苦豆子种子中提取生物碱，最佳提取条件为料液比1∶30，pH 1.5，提取时间5h。使用大孔树脂吸附法对提取的生物碱进行纯化，考察了SP850、SP825、SP700、SP207、AB-8等5种树脂的吸附效果，其中SP850型树脂吸附量和解析量均最大，分别为27.4mg/mL和20.4mg/mL。测定了体积分数为50%、60%、70%的乙醇洗脱效果，确定了60%乙醇为最佳洗脱浓度，洗脱体积为6倍柱体积。经氯仿萃取和旋转蒸发，得到纯度达83.5%的生物碱粗产品。运用硅胶柱层析技术从生物碱粗品中分离生物碱单体，考察了氯仿-甲醇-氨水系统，正己烷-乙醇-氨水系统，丙酮-甲醇-氨水系统在硅胶薄层色谱上对生物碱的分离效果，确定以V_正己烷∶V_乙醇∶V_氨水=8∶2∶0.1作为流动相。收集洗脱液，经过结晶和重结晶，得到苦参碱和槐定碱晶体。经检测，苦参碱纯度为98.3%，槐定碱纯度达96.8%。

Isolation and purification of matrine and sophoridine from the seeds of Sophora alopecuroides

Processes for the isolation and purification of matrine and sophoridine from the seeds of Sophpra alopecuroides have been studied.Using acidic water to extract total alkaloids from the seeds of Sophpra alopecuroides,the optimal extraction conditions were found to be:a solid to liquid ratio of 1∶30,pH of 1.5 and extraction time of 5 h.Macroporous resins were employed to purify the total alkaloids from Sophpra alopecuroides.In the static state,SP850 resin possessed the maximum adsorption capability(27.4 mg/mL) and desorption capability(20.4 mg/mL) of all the macroporous resins tested(SP850,SP825,SP700,SP207 and AB-8).By comparison of the elution effects of 50%,60% and 70% ethanol,60% ethanol was found to be the most suitable eluant,and the appropriate elution volume was 6 bed volumes.After extracting the alkaloids by chloroform and rotary evaporation to remove chloroform,the purity of the alkaloids reached 83.5%.Monomeric alkaloids were further separated from total alkaloids by silica gel column chromatography.Based on a comparison of the separation effects of chloroform-methanol-ammonia systems,n-hexane-ethanol-ammonia systems and acetone-methanol-ammonia systems on a silica gel column,Vn-hexane∶Vethanol∶Vammonia=8∶2∶0.1 was found to be the best mobile phase.Crystals of matrine and sophoridine were obtained through collecting the respective eluants,crystallization and recrystallization.By HPLC analysis,the purity of matrine reached 98.3%,and that of sophoridine was 96.8%.