艾纳香叶中花椒油素的制备  

Preparation of xanthoxylin from leaves of Blumea balsamifera( L. ) DC.

作　　者：王远辉[1] 宋燕燕[1] 

机构地区：[1]河南工业大学粮油食品学院

出　　处：《食品与发酵工业》2015年第1期131-135,共5页Food and Fermentation Industries

基　　金：国家科技型中小企业技术创新基金(11C26215205838);贵州省科技型中小企业技术创新基金(黔科合字2011[5002]号)

摘　　要：提出从艾纳香叶中制取花椒油素的方案。通过同时蒸馏萃取法(SDE)提取花椒油素,利用硅胶柱层析分离粗品,经过重结晶纯化得高纯产品,通过气相色谱(GC)和核磁共振(NMR)对花椒油素进行定量和定性分析。在料水比1∶8,溶剂(无水乙醚)体积60 m L,提取时间2.5 h的参数下通过SDE法提取花椒油素,GC测定显示粗提物中含量达20.26%。硅胶柱参数为洗脱液配比[V(乙酸乙酯)∶V(石油醚)=1∶19]、径高比1∶14、样品与硅胶质量比(上样量)1∶40、洗脱液流速3.5 m L/min时,可分离到花椒油素粗品(纯度72.09%),回收率为99.04%。经过3次重结晶得到高纯度产品(98.37%),总回收率为91.92%,得率为0.28%。NMR结果证实产品为花椒油素。The preparation of high-purity xanthoxylin from Blumeabalsamifera （L.） DC. Leaves was studied. Xanthoxylin was extracted by simultaneous distillation extraction （SDE） , and crude product was isolated by silica gel column, and high-purity product was obtained by recrystallization. Gas chromatography （GC） and nuclear magnetic resonance （NMR） were used for quantitative and qualitative analysis. Xanthoxylin was extracted by SDE with parame- ters （ratio of material to water = 1 ： 8, solvent volume 60 mL, extraction time 2.5 h） , and GC analysis showed that xanthoxylin content of crude extract was 20.26%. Crude xanthoxylin was isolated by silica gel column with the param- eters of eluent ratio （ ethyl acetate： petroleum ether ） 1 ： 19, ratio of diameter to height 1 ： 14, ratio of sample to silica gel 1：40, eluent rate 3.5 mL/min. The purity of xanthoxylin was 72.09% , and the recovery was 99.04%. Finally, high-purity xanthoxylin（98. 37% ） was obtained by recrystallization for three times, and the total recovery was 91.92% , and the yield was 0.28%. NMR confirmed that the isolated crystal was xanthoxylin. The method was used to prepare high-purity xanthoxylin with high-recovery from leaves of B. balsamifera. It provided reference for future industrial application.

关 键 词：艾纳香 花椒油素 气相色谱 核磁共振 制备 

分 类 号：TS264[轻工技术与工程—发酵工程]