花椒油素的纯化和鉴定.pdf

现代食品科技 Modern Food Science and Technology 2015, Vol.31, No.1 花椒油素的纯化和鉴定 孙克奎 （黄山学院旅游学院，安徽黄山 245021） 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。 关键词：花椒；花椒油素；高效液相色谱；同时蒸馏萃取；硅胶；重结晶；核磁共振 文章篇号：1673-9078(2015)1-137-141 DOI: 10.13982/j.mfst.1673-9078.2015.1.025 Purification and Identification of Xanthoxylin SUN Ke-kui (Tourism College, Huangshan University, Huangshan 245021, China) 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 conte