摘 要：一种筛选适当的高速逆流色谱条件以实现功劳叶正丁醇段化合物的快速分离的方法已经建立起来。采用D-101大孔吸附树脂对功劳叶中的物质进行洗脱富集。利用高效液相色谱法结合薄层色谱法分析优化溶剂体系，选择乙酸乙酯-正丁醇-水（1:2:3）为HSCCC溶剂系统，上相为固定相，下相为流动相，主机转速为800 r/min，体积流量为2 mL/min，检测波长为254 nm。所接收馏分通过旋转蒸发浓缩。最终得到四种正丁醇段功劳叶的单体。结论：通过HSCCC法快速分离功劳叶正丁醇段化合物，得到单体，以便于对各种化合物单体进行物质结构鉴定和活性研究。70576

毕业论文关键字：高速逆流色谱，高效液相色谱，大孔树脂，阔叶十大功劳

Abstract： A rapid approach to filtering the appropriate conditions to separate compounds from the BuOH fraction of the leaves of Mahonia bealei by high-speed counter-current chromatography(HSCCC) has been established. Compounds of the leaves of M. bealei were enriched with D101 macropoous resin. HPLC and TLC were used to analyze and optimize the solvent system and the two-phrase solvent system ethyl acetate-n-butanol-water (1:2:3) was selected. The upper phrase was used as the stationary phrase and the lower phrase was used as the mobile phrase with flow rate of 2 mL/min, the revolution speed was set at 800 r/min, and detected at 254 nm. The fractions were gathered by rotary evaporator. Finally, four kinds of compounds were obtained. Conclusion:HSCCC with solvent system of ethyl acetate-n-butanol-water (1:2:3) was confirmed to be a rapid and efficient tool for the separation of M. bealei for the preparation to identify the structures of these compounds.

Keywords: High-speed Countercurrent Chromatography,HPLC, macroporous resin, M. bealei

目 录

1 绪论 1

1.1 高速逆流色谱 1

1.1.1 高速逆流色谱简介 1

1.1.2高速逆流色谱的特点 2

1.1.3高速逆流色谱在天然产物分离纯化中的应用 2

1.2 高速逆流色谱的溶剂体系 2

1.2.1 溶剂体系选择原则 2

1.2.2 溶剂体系选择方法 2

1.3 阔叶十大功劳 3

1.3.1阔叶十大功劳简介 3

1.3.2阔叶十大功劳的现代研究进展 3

2 仪器与材料 3

3 方法与结果 3

3.1 HPLC条件 3

3.2 粗提物的准备 3

3.3分配系数的测定 5

3.4两相溶剂系统的选择 5

3.5目标成分的分离制备 6

4结果与讨论 7

结论 9

参考文献 10

致 谢 12

1 绪论

大孔吸附树脂是一种新型有机高分子吸附剂，且理化性质稳定，能够选择性吸附有机物[1]，具有吸附量大，安全可靠，可重复利用等优点，近年来广泛用于分离纯化中草药中的有效成分。刘小雪等人[2]通过比较AB-8、D-101、HPD-400三种大孔吸附树脂对桑叶总黄酮吸附率与解吸率，筛选出最好性能的树脂为D-101，并且确定了其纯化桑叶黄酮的最佳工艺条件。术合塔尔·吐尔洪等人[3]对11中大孔吸附树脂进行了比较，采用静态吸附方法筛选出纯化最适合于昆仑雪菊中总黄酮的树脂是NAK-9树脂，同时确定了其最佳吸附条件，为昆仑雪菊黄酮类物质的分离和鉴定打下了基础。