香荚兰豆中香兰素葡萄糖苷的提取、分离及表征  

Extraction,separation and characterization of vanillin glucoside from vanilla beans

作　　者：杨峰 黄申 席高磊 陈芝飞 于国强 付瑜锋 蔡莉莉 樊新顺 赵志伟 李杰 王小飞 王东 YANG Feng;HUANG Shen;XI Gaolei;CHEN Zhifei;YU Guoqiang;FU Yufeng;CAI Lili;FAN Xinshun;ZHAO Zhiwei;LI Jie;WANG Xiaofei;WANG Dong(Henan Cigarette Industry Tobacco Sheet Co.,Ltd.,Xuchang 461000,Henan,China;School of Food and Biological Engineering,Zhengzhou University of Light Industry,Zhengzhou 450002,China;Technology Center,China Tobacco Henan Industrial Co.,Ltd.,Zhengzhou 450016,China)

机构地区：[1]河南卷烟工业烟草薄片有限公司,河南省许昌市461000 [2]郑州轻工业大学食品与生物工程学院,郑州450002 [3]河南中烟工业有限责任公司技术中心,郑州市450016

出　　处：《烟草科技》2020年第8期44-49,共6页Tobacco Science & Technology

基　　金：河南中烟工业有限责任公司科技项目“加热不燃烧卷烟中单体香料释放行为及其功能评价”(AW2019001)。

摘　　要：为进一步拓展天然香兰素的开发途径,采用超声辅助溶剂萃取法从香荚兰豆中提取了香兰素葡萄糖苷粗提物,以香兰素葡萄糖苷提取率为指标,通过单因素试验和正交试验对粗提物提取工艺进行了优化,并利用制备高效液相色谱技术分离获得了香兰素葡萄糖苷单体。结果表明:①粗提物最佳提取工艺为萃取时间10 min、萃取温度65℃、固液比1∶11、萃取功率140 W,在此条件下香兰素葡萄糖苷提取率为1.88%;②当流动相中0.5%(质量分数)乙酸水溶液和甲醇比例为80∶20(体积比)时,利用制备高效液相色谱可有效分离纯化香兰素葡萄糖苷,产品得率为1.36%;③采用1H NMR和13C NMR对产品进行结构表征,进一步验证了所得产品为目标化合物香兰素葡萄糖苷。该提取分离工艺处理量较大、步骤简便、成本低廉,可为天然香兰素葡萄糖苷单体开发提供参考。In order to expand the application of natural vanillin,the crude product of vanillin glycoside was extracted from vanilla beans by ultrasonic assisted solvent extraction.The extraction process was optimized by a single factor test and orthogonal test with extraction rate as the index,and vanillin glucoside monomer was separated by high performance liquid chromatography.The results showed that:1)The optimal extraction conditions for the crude product were:10 min extraction time,65℃extraction temperature,a solid to liquid ratio(mass ratio)1∶11,and 140 W extraction power.Under these conditions,the extraction rate of vanillin glucoside was 1.88%.2)When the ratio of acetic acid aqueous solution(mass percentage 0.5%)to methanol in the mobile phase was 80∶20(v/v),vanillin glucoside monomer was effectively separated by the preparation high performance liquid chromatography with a product yield of 1.36%.3)The structure of vanillin glycoside was characterized by 1H NMR and 13C NMR,which confirmed that the obtained product was vanillin glucoside.The extraction and separation processes had the advantages of a high processing capacity,simpler steps and lower cost,thus providing a reference for the development of natural vanillin glucoside。

关 键 词：香兰素葡萄糖苷 香荚兰豆 提取 分离 表征 工艺优化 

分 类 号：TQ656.5[化学工程—精细化工]