超临界CO_2提取油橄榄叶中橄榄苦苷及其结构鉴定

Extraction and Structure Identification of Oleuropein from Olea europaea Leaves by Supercritical Carbon Dioxide Extraction Technology

采用超临界CO2萃取技术提取油橄榄叶,提取液经硅胶柱层析分离得到质量分数为96%以上的单体,通过液质联用分析(HPLC-MS)、核磁共振(1H NMR)和红外(IR)鉴定该组分为橄榄苦苷。采用C18色谱柱,紫外检测波长为254 nm,甲醇/水体积比40∶60为流动相,流速0.5 m L/min,建立橄榄苦苷的HPLC分析方法。通过单因素和正交试验研究,得到萃取优化条件为:萃取压力25 MPa,萃取温度45℃,分离温度45℃,萃取时间4 h,CO2流量30 kg/h。在此条件下,橄榄苦苷得率为0.435%。

The Olea europaea leaves were extracted by supercritieal carbon dioxide extraction technology, then the extract was analyzed by silica gel column chromatography. A compound was isolated from the extract with content of 96% which was identified as oleuropein by HPLC-MS, 1H NMR, and IR. The HPLC analysis was carried out with column Cls and MeOH-water 40 ： 60 （ volume ratio） as mobile phase at flow rate 0.5 mL/min, and monitored at 254 nm. By single factor and orthogonal experiments, optimal extraction conditions were obtained as follows： extraction pressure 25 MPa, extraction temperature 45 ℃, separation temperature 45 ℃, extraction time 4 h, and CO2 flow rate 30 kg/h. At the optimal extraction conditions, the yield of oleuropein was 0. 435%.