超临界CO2提取油橄榄叶中橄榄苦苷及其结构鉴定

doi:10.3969/j.issn.0253-2417.2015.02.011

林产化学与工业 ›› 2015, Vol. 35 ›› Issue (2): 73-78.doi: 10.3969/j.issn.0253-2417.2015.02.011

超临界CO₂提取油橄榄叶中橄榄苦苷及其结构鉴定

郭玉玉¹, 王玲¹, 罗金岳¹, 邵双喜¹, 王成章², 刘祖广³

1. 南京林业大学化学工程学院;江苏省生物质绿色燃料与化学品重点实验室, 江苏南京 210037;
2. 中国林业科学研究院林产化学工业研究所, 江苏南京 210042;
3. 广西林产化学与工程重点实验室, 广西南宁 530006

收稿日期:2014-01-07 出版日期:2015-04-25 发布日期:2015-04-24
通讯作者: 罗金岳(1964-),男,浙江余姚人,教授,研究方向为林产化学加工工程;E-mail:luojinyue@njfu.com.cn。 E-mail:luojinyue@njfu.com.cn
作者简介:郭玉玉(1989-),女,山西孝义人,硕士生,研究方向:天然产物化学;E-mail:gyy879117557@163.com
基金资助:
广西林产化学与工程重点实验室重点项目(GXFC13-01); 江苏高校优势学科建设工程资助项目(无编号)

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

GUO Yu-yu¹, WANG Ling¹, LUO Jin-yue¹, SHAO Shuang-xi¹, WANG Cheng-zhang², LIU Zu-guang³

1. College of Chemical Engineering, Nanjing Forestry University;Jiangsu Key Lab of Biomass-based Green Fuels and Chemicals, Nanjing 210037, China;
2. Institute of Chemical Industry of Forest Products, CAF, Nanjing 210042, China;
3. Guangxi Key Laboratory of Chemistry and Engineering of Forest Products, Nanning 530006, China

Received:2014-01-07 Online:2015-04-25 Published:2015-04-24

摘要/Abstract

摘要： 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 mL/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%。

关键词: 油橄榄叶, 超临界CO₂萃取, 橄榄苦苷, 提取工艺, 化学结构

Abstract: The Olea europaea leaves were extracted by supercritical 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 C₁₈ 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%.

Key words: Olea europaea leaves, supercritical carbon dioxide extraction, oleuropein, extraction technology, chemical structure

中图分类号:

TQ35

郭玉玉, 王玲, 罗金岳, 邵双喜, 王成章, 刘祖广. 超临界CO₂提取油橄榄叶中橄榄苦苷及其结构鉴定[J]. 林产化学与工业, 2015, 35(2): 73-78.

GUO Yu-yu, WANG Ling, LUO Jin-yue, SHAO Shuang-xi, WANG Cheng-zhang, LIU Zu-guang. Extraction and Structure Identification of Oleuropein from Olea europaea Leaves by Supercritical Carbon Dioxide Extraction Technology[J]. Chemistry and Industry of Forest Products, 2015, 35(2): 73-78.

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超临界CO₂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

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