College of Chemistry & Pharmacy, Northwest A&F University, Yangling, China.
Life Science Research Core Services, Northwest A&F University, Yangling, China.
J Sep Sci. 2024 Jul;47(13):e2400234. doi: 10.1002/jssc.202400234.
In this study, we employed a combination approach for the preparative separation of constituents from Ginkgo biloba L. leaves. It involved multi-stage solvent extractions utilizing two-phase multi-solvent systems and countercurrent chromatography (CCC) separations using three different solvent systems. The n-heptane/ethyl acetate/water (1:1:2, v/v) and n-heptane/ethyl acetate/methanol/water (HepEMWat, 7:3:7:3, v/v) solvent systems were screened out as extraction systems. The polarities of the upper and lower phases in the multi-solvent systems were adjustable, enabling the effectively segmented separation of complex constituents in G. biloba L. The segmented products were subsequently directly utilized as samples and separated using CCC with the solvent systems acetate/n-butanol/water (4:1:5, v/v), HepEMWat (5:5:5:5, v/v), and HepEMWat (9:1:9:1, v/v), respectively. As a result, a total of 11 compounds were successfully isolated and identified from a 2 g methanol extract of G. biloba L through two-stage extraction and three CCC separation processes; among them, nine compounds exhibited high-performance liquid chromatography purity exceeding 85%.
在这项研究中,我们采用组合方法从银杏叶中制备性分离成分。它涉及利用两相多溶剂系统进行多阶段溶剂萃取和使用三种不同溶剂系统进行逆流色谱(CCC)分离。正庚烷/乙酸乙酯/水(1:1:2,v/v)和正庚烷/乙酸乙酯/甲醇/水(HepEMWat,7:3:7:3,v/v)溶剂系统被筛选为萃取系统。多溶剂系统中上下相的极性是可调的,能够有效地分段分离银杏叶中复杂的成分。分段产物随后直接用作样品,并分别使用溶剂系统乙酸乙酯/正丁醇/水(4:1:5,v/v)、HepEMWat(5:5:5:5,v/v)和 HepEMWat(9:1:9:1,v/v)进行 CCC 分离。结果,通过两步提取和三次 CCC 分离过程,从 2 g 银杏叶甲醇提取物中成功分离并鉴定出 11 种化合物;其中 9 种化合物的高效液相色谱纯度超过 85%。