微波辅助萃取-大孔树脂分离纯化芳樟叶黄酮

Separation and purification of flavonoids from Cinnamomum camphora leaves via microwave-assisted extraction and macroporous resin adsorption

为了综合利用芳樟叶精油提取过程中产生的大量残渣,该文利用微波辅助萃取和大孔树脂选择性吸附来分离纯化芳樟叶黄酮。采用L9(34)正交试验,考察了萃取剂、微波辐射功率、辐射时间及料液比对黄酮得率的影响,确定了微波辅助萃取的优化工艺条件:以60%乙醇做萃取剂,微波功率320W,间歇辐射2次,每次1min,料液质量体积比1:12,在此条件下,芳樟叶黄酮的提取得率为2.97%,与乙醇热回流提取方法相比,得率提高了6.83%,时间缩短了98.89%;为进一步纯化萃取所得的黄酮提取物,选择6种大孔吸附树脂,测定芳樟叶黄酮在树脂上的吸附量和解吸率,筛选出了吸附剂HPD-450,其对芳樟叶黄酮有较好的静态吸附和解吸效果。经装填有大孔树脂HPD-450的固定床纯化后黄酮纯度由22.49%提高到51.28%,纯化倍数2.3倍。

Flavonoids was extracted by the microwave-assisted extraction technology from the residue of Cinnamomum camphora leaves during essential oil extraction.Macroporous resin adsorption was used for further purification.With orthogonal designed experiments the optimal extraction conditions were determined:60%ethanol aqueous solution, microwave power 320 W and treated for 2 min,1﹕12(g·mL -1 )for the mass to volume ratio of material to extractant. Under such conditions,the yield of the flavonoids reached 2.97%,which is 6.83%higher than that obtained using heat ethanol reflux extraction,and the operation duration of the newly developed extraction technology was significantly reduced by 98.89%.Six kinds of macroporous resin were then examined for further purification of Cinnamomum camphora flavonoids.Results showed that HPD-450 resin possessed correspondingly the best absorption and desorption behavior.After an absorption-desorption operation applied upon an HPD-450 resin packed column,the purity of flavonoids could be improved to 51.3%from 22.5%,and the purification fold is 2.3.