花椒油素的纯化和鉴定

Purification and Identification of Xanthoxylin

研究了从花椒中提取制备高纯花椒油素的方案。采用同时蒸馏萃取(SDE)提取花椒油素,利用硅胶柱色谱分离得到粗品,经过重结晶纯化得高纯花椒油素,利用核磁共振(NMR)和反相高效液相色谱(RP-HPLC)进行定性和定量分析。在SDE过程中,料水比为1:10,溶剂(无水乙醚)用量为60 m L,提取时间为1.5 h时,粗提物中花椒油素含量达47.26%。以洗脱液配比(乙酸乙酯:石油醚)为1:15、径高比为1:12、样品与硅胶质量比(上样量)为1:40、洗脱液流速为4 m L/min的硅胶柱分离得到花椒油素粗品(纯度81.79%),回收率达99.12%。最后通过重结晶获得高纯花椒油素(纯度98.23%),总回收率达90.63%,得率为0.88%。NMR分析证实晶体确为花椒油素。该方案可实现从花椒中高回收地制取高纯花椒油素,为拓宽花椒的精深加工提供参考。

The aim of this work was to study an approach for the preparation of high-purity xanthoxylin from Zanthoxylum bungeanum Maxim. Xanthoxylin was extracted by simultaneous distillation extraction （SDE）, crude xanthoxylin was isolated using a silica gel column, and high-purity xanthoxylin was obtained by recrystallization. Nuclear magnetic resonance （NMR） and reversed phase high performance liquid chromatography （RP-HPLC） were used for qualitative and quantitative analysis, respectively. During the SDE, the following conditions were used： material to water ratio 1： 10; solvent volume 60 mL; extraction time 1.5 h. RP-HPLC analysis showed that the xanthoxylin content in the crude extract was 47.26%. Crud xanthoxylin was isolated using a silica gel column under the following conditions： eluent ratio （ethyl acetate： petroleum ether） 1： 15; diameter to height ratio 1：12; sample to silica gel ratio 1：40; eluent rate 4 mL/min. The purity of the isolated xanthoxylin was 81.79% and the recovery was 99.12%. Finally, high-purity xanthoxylin （98.23%） was obtained by recrystallization; the total recovery was 90.63% and the yield was 0.88%. NMR analysis showed that the isolated crystal was xanthoxylin. Thus, this approach could achieve the preparation of high-purity xanthoxylin, with high-recovery, from the leaves of Zanthoxylum bungeanum and serve as a reference for broadening the scope ofZanthoxylum bungeanum deep-processing.