第 49 卷第 4 期Vol. 49 No. 4
2019 年 8 月Aug 2019

所属栏目:医药及中间体

6-姜酚的制备与结构表征
凌 琳,李英奇,邓珊霞,曾健青* (湖南和广生物科技有限公司,湖南 永州 425000)
摘 要:以超临界二氧化碳萃取所得的姜树脂为原料,采用连续液-液萃取法制得6-姜酚粗品,再经过加压硅胶柱层析法,对其进行分离纯化,得到含量为95%以上的6-姜酚,通过质谱与核磁共振波谱对其进行结构表征。考察原料中6-姜酚含量、硅胶目数、操作温度、洗脱溶剂流速等对6-姜酚柱层析分离效果的影响。结果表明,在层析硅胶目数为200~300目、操作温度为10℃、洗脱溶剂的流速为1.35 mL·cm-2·min-1、6-姜酚粗品中6-姜酚含量为64.32%的条件下,进行加压柱层析,制备得到含量为95.12%的6-姜酚,6-姜酚的回收率81.46%。
关键词:6-姜酚;姜树脂;加压硅胶柱层析法;结构表征
中图分类号:R284  文献标识码:A  文章编号:1009-9212(2019)04-0035-06
Preparation and Structural Characterization of 6-Gingerol
LING Lin, LI Ying-qi, DENG Shan-xia, ZENG Jian-qing* (Hunan Health-Guard Biotechnology Incorporated Company, Yongzhou 425000, China)
Abstract:Using ginger oleoresin as the raw materia extracted from ginger by supercritical carbon dioxide extraction method, 6-gingerol with a purity of more than 95% was prepared efficiently through separation and purification by continuous liquid-liquid extraction and pressurized silica gel column chromatography. The obtained 6-gingerol was characterized by mass spectrometry and nuclear magnetic resonance spectroscopy. The effects of factors including the content of 6-gingerol in raw materials, the size of silica gels, operating temperature and the flow rate of elute on the separation efficiency of 6-gingerol were evaluated. The results showed that 6-gingerolwith a purity of 95.12% could be obtained rapidly with a yield of 81.47% under the following conditions: that the purity of 6-gingerol as raw material for pressurized silica gel column chromatography was of 64.32%; the size of silica gel was of 200~300 mesh; operating temperature was of 10℃ and the elute flow rate was of 1.35 mL·cm-2·min-1 for a gradient elution.
Key words:6-gingerol; ginger oleoresin; pressurized silica gel column chromatography; structural characterization
基金项目:湖南省创新创业技术投资项目(2017GK5038),湖南省企业科技创新创业团队项目(和广生物现代萃取分离与应用科技创新创业团队)。
作者简介:凌 琳(1991-),女,湖南株洲人,硕士,研究方向:植物提取、分离纯化与应用(E-mail:18874848142@163.com)。
联 系 人:曾健青,博士,研究员,研究方向:超临界流体技术研究与应用(E-mail:jackingzeng@vip.163.com)。
收稿日期:2019-08-06