艾纳香叶中花椒油素的制备

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 mL,提取时间2.5h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 mL/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 parameters (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 parameters 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.