花椒油素的纯化和鉴定

Purification and Identification of Xanthoxylin

摘要:

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 mL，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 mL/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。

Abstract:

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%. Crude 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 of Zanthoxylum bungeanum deep-processing.