油橄榄中橄榄苦苷的提取及纯化工艺研究

采用ODS C18色谱柱,流动相为甲醇:水(0.2%醋酸)体积比45:55,检测波长为230 nm,建立油橄榄叶中橄榄苦苷的HPLC分析方法。采用单因素和正交试验筛选优化油橄榄叶橄榄苦苷浸提的最佳工艺,并进一步研究大孔树脂静态和动态吸附和解吸附性能。结果表明:1)热回流浸提的最佳工艺为乙醇体积分数80%,温度70℃,提取时间3.5 h,料液比1:15(g:mL),提取次数2次。2)通过对比不同树脂对橄榄苦苷的吸附,筛选出选择性吸附好的AB-8树脂,吸附量为每克湿树脂32.1 mg。AB-8树脂纯化的最佳条件为:上样质量浓度为2 g/L,70%乙醇-水洗脱,流速为3 mL/min,洗脱液用量为3 BV。3)橄榄苦苷的粗提物经过AB-8树脂纯化后,橄榄苦苷的纯度达到47.90%,黄酮含量为16.4%,收率为6.43%。

Extraction of Oleuropein from Olive Leaves and Its Purification

Oleuropein was analysized by HPLC with ODS C18 column, using volume ratio of methanol to water of 45:55 as mobile phase under UV light of 230 nm. Oleuropein composition were extracted by hot reflux extraction, using experimental design of single factor and orthogonal test. Different kinds of macropore resins were applied to test capability of absorption and desorption of oleuropein under static and dynamic state. The results indicate that 1)the optimum extraction conditions were as follows: 80% ethanol volume fraction, temperature 70℃,extraction time 3.5 h, solid-liquid ratio 1:15(g:mL), extract 2 times; 2) The best resin was AB-8 with a 32.1 mg/g absorption capability. The optimal desorption conditions were sample mass concentration 2 g/L, 70% ethanol-water eluting, flow rate 3 mL/min, 3 BV eluent dose; 3) The purification of oleuropein reached 47.90% from the raw extract of olive leaves. Total flavonoids was 16.4% and the yield was 6.43% after AB-8 purification.