期刊
JOURNAL OF CHROMATOGRAPHY A
卷 1406, 期 -, 页码 224-230出版社
ELSEVIER
DOI: 10.1016/j.chroma.2015.06.038
关键词
Countercurrent chromatography; Aralia continentalis; Diterpenoid; Distribution ratio; Three-phase solvent system
资金
- Ministry of Food and Drug Safety for Research on the Preparation of Reference Compounds of Natural Products (I [13172MFDS417]
- National Research Foundation [MRC2009-93146]
Aralia continentalis (Araliaceae) is widely used as a medicinal plant in East Asia. Previous studies have indicated that diterpenoid isomers (kaurenoic acid, continentalic acid, and ent-continentalic acid) are the major bioactive compounds of this plant. A new strategy was developed to alleviate difficulties in the separation of these isomers from this plant. A three-phase solvent system was applied to separate the isomers, and furthermore, the distribution ratio (K-c) was introduced as a substitute for the partition coefficient (K-D). For compounds exhibiting a single equilibrium, their distributions in two immiscible phases were only affected by the partition coefficient of each solute. However, compounds that have a dissociating functional group (e.g., -COOH) are involved in two types of equilibrium in the two-phase system. In this case, the partitioning behaviors of the solutes are greatly affected by the pH of the solution. A mathematical prediction was applied for adjusting the solutions to the proper pH values. To prevent non-used phase (medium phase) waste, both the stationary phase (upper phase) and mobile phase (lower phase) were prepared on-demand without pre-saturation with the application of H-1 NMR. Each fraction obtained was collected and dried, yielding the following diterpenoid isomers from the 50 mg injected sample: kaurenoic acid (19.7 mg, yield: 39%) and ent-continentalic acid (21.3 mg, yield: 42%). (C) 2015 Elsevier B.V. All rights reserved.
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