草木樨药材中香豆素类化合物提取分离纯化研究

Study on the extraction,isolation and purification of coumarin in Melilotus suaveolens Ledeb

目的:建立草木樨药材中主要活性成分香豆素类化合物工业化提取分离纯化方法与条件。方法:通过比较不同的提取条件;有机溶剂萃取法与大孔树脂分离纯化,采用HPLC法测定香豆素。结果:药材最佳提取工艺:取草木樨药材粗粉,加50%乙醇回流提取3次,每次提取1.0h,溶媒用量依次为20,15,12倍。纯化最佳工艺:选用YWD07D1型大孔吸附树脂,为200g药材/L溶液,上样树脂柱径高比为1∶7,药材和树脂用量比为7∶1。上样后先用3倍柱体积去离子水洗脱,再用3倍柱体积80%乙醇洗脱。收集80%乙醇洗脱液,50℃减压浓缩。结论:总有效部位以香豆素计含量达到50%以上。

OBJECTIVE To explore the extraction and purification method for coumarin from Melilotus suaveolens Ledeb. METHODS To compare different extraction methods, different purifying conditions of solvents extraction and macroporous resin. RESULTS The results showed that the optimum extraction conditions were： adding 50% ethanol to extract for three times, 1.0 h each time, the amounts of added ethanol were 20 times, 15 times and 12 times, respectively. Best process： The optimum purifying process was as follows： the best macroporous resin was YWD07D1, the sample concentration was 200 g·L^-1, the ratio of cloumn diameter to cloumn height was 1 ： 7, the ratio of herb weight to macroporous resin weight was 7： 1.The sample was washed with 3 bed volume （BV）of distilled water, then eluted with 3 BV of 80% ethanol, yield of eoumarin was 90%. CONCLUSION product purity was above 50%.