金银花叶同步提取物总黄酮和绿原酸分离纯化研究

Study on the Separation and Purification of Total Flavonoids and Chlorogenic Acid in the Synchronous Extraction of Honeysuckle Leaves

研究了乙酸乙酯萃取、大孔树脂分离纯化金银花叶绿原酸和总黄酮的工艺。以金银花叶加压同步提取液为试验样品,经乙酸乙酯萃取,乙酸乙酯层、水层产物分别使用AB-8树脂和D101B树脂分离纯化。结果表明,乙酸乙酯萃取,可以将脂溶性黄酮和水溶性黄酮、绿原酸分离,乙酸乙酯层脂溶性黄酮,遴选出最佳纯化大孔树脂为AB-8树脂,单因素试验优选的工艺参数:上样液pH值为4.0、质量浓度为2.0 mg/mL、流速为2.0 BV/h;解吸液为体积分数80%乙醇溶液、解吸液流速为2.0 BV/h、解吸液体积7.0 BV;水层采用D101B树脂分离纯化绿原酸和总黄酮。同步提取液中绿原酸和总黄酮得到较好地分离和纯化,二步法分离纯化后的产物,绿原酸收率为89.71%,纯度达到61.22%;总黄酮收率为93.45%,纯度达到78.92%。

The process of ethyl acetate extraction and separation and purification of chlorogenic acid and total flavonoids from honeysuckle leaves by macroporous resin was studied.Using the pressurized synchronous extraction solution of honeysuckle leaves as the experimental sample,after ethyl acetate extraction,the ethyl acetate layer and water layer products were extracted and purified using AB-8 resin and D101B resin respectively.The results showed that ethyl acetate extraction can separate lipid-soluble flavonoids from water-soluble flavonoids and chlorogenic acid.The ethyl acetate layer of lipid-soluble flavonoids,AB-8 resin was selected as the best purification macroporous resin.Preferred process parameters for single-factor testing:pH of the sample solution was 4.0,concentration of the sample solution was 2.0 mg/mL,flow rate of the sample solution was 2.0 BV/h,desorption solution was 80%ethanol solution,desorption flow rate was 2.0 BV/h,and desorption volume was 7.0 BV;The water layer uses D101B resin to separate and purify chlorogenic acid and total flavonoids.The chlorogenic acid and total flavonoids in the synchronous extraction solution were well separated and purified.After the two-step separation and purification of the product,the yield of chlorogenic acid was 89.71%,and the purity reached 61.22%;The total flavonoid yield is 93.45%,and the purity reaches 78.92%.