硅胶柱层析法分离纯化杜仲粕中桃叶珊瑚苷-食品科学.pdf

58 2010, Vol. 31, No. 14 食品科学 ※工艺技术 1,2 1 1 1,2 李 辉 ，汪 兰 ，彭玉丹 ，张永康 (1.吉首大学生物资源与环境科学学院，湖南 吉首 416000 ； 2.吉首大学 林产化工工程湖南省重点实验室，湖南 张家界 427000) 探讨使用硅胶柱层析法从杜仲粕中分离纯化桃叶珊瑚苷(Au)，优化柱层析吸脱附条件，用薄层色谱法(TLC) 和高效液相色谱法(HPLC)对产品进行定性定量分析。结果表明：优化的硅胶用量为生药质量的 2 倍，使用 V( 甲醇): V(氯仿): V(石油醚): V(乙酸乙酯)为7:1:0.5:1.5 的混合溶剂在1.0mL/min流速下进行洗脱，通过收集含Au 高的组分，经 减压浓缩、结晶、过滤、重结晶等过程，可获纯度为 96.56% 的桃叶珊瑚苷产品。 桃叶珊瑚苷；柱层析；硅胶；纯化 Purification of Aucubin from the Crude Extract of Eucommia ulmoides Seeds by Silica Gel Chromatography 1,2 1 1 1,2 LI Hui ，WANG Lan ，PENG Yu-dan ，ZHANG Yong-kang (1. College of Biology and Environmental Science, Jishou University, Jishou 416000, China ；2. Hunan Provincial Key Laboratory of Forest Products and Chemical Industry Engineering, Jishou University, Zhangjiajie 427000, China) Abstract ：A silica gel chromatographic method was presented for the purification of aucubin (Au) from the crude extract of the residue of Eucommia ulmoides seed meal left after linolenic acid extraction. Subsequently, the extracted product was analyzed qualitatively and quantitatively. An optimal purification of Au was achieved by using a 2-fold mass of silica gel for Au adsorption followed by desorption with a 70% methanol/chloroform/petroleum ether/ethyl acetate mixture (7:1:0.5:1.5, V/V) at a flow rate of 1.0 mL/min. The eluate fractions were harvested and subjected to vacuum condensation, crystallization, filtration and recrystallization, and a final Au product with 96.56% purity was obtained. Key words ：aucubin ；column chromatography ；silica gel ；purification 中图分类号：TS201.1 ；R284.2 文