Abstract
A high-speed counter-current chromatography (HSCCC) method was established for the preparative separation of three sesquiterpenoid lactones from Eupatorium lindleyanum DC. The two-phase solvent system composed of n-hexane–ethyl acetate–methanol–water (1:4:2:3, v/v/v/v) was selected. From 540 mg of the n-butanol fraction of Eupatorium lindleyanum DC., 10.8 mg of 3β-hydroxy-8β-[4'-hydroxy-tigloyloxy]-costunolide, 17.9 mg of eupalinolide A and 19.3 mg of eupalinolide B were obtained in a one-step HSCCC separation, with purities of 91.8%, 97.9% and 97.1%, respectively, as determined by HPLC. Their structures were further identified by ESI-MS and 1H-NMR.
Highlights
Eupatorium lindleyanum DC. is a traditional Chinese herb
There is no report on the use of High-speed counter-current chromatography (HSCCC) for the isolation and purification of sesquiterpenoid lactones from Eupatorium lindleyanum DC, we report an efficient method for the preparative isolation and purification of three sesquiterpenoid lactones from Eupatorium lindleyanum DC. by one-step HSCCC
The results indicated that the solvent system of n-hexane–ethyl acetate–methanol–water at the volume ratios of 2:4:3:2 (v/v/v/v) had small K values for the three compounds, and the solvent system n-hexane–ethyl acetate–methanol–water (1:4:3:3, v/v/v/v) provided suitable K values for separating compounds 2 (K value: 0.61) and 3 (K value: 1.26) but was unsuitable for compound 1 (K value: 0.26)
Summary
Eupatorium lindleyanum DC. (family Compositae) is a traditional Chinese herb. Its aerial part, called ‘Yemazhui’, shows antihistaminic, antibacterial and antioxidant activities [1,2,3], and is traditionally used for the treatment of inflammation and asthma, as well as throat disorders [1]. The sesquiterpenoid lactones, which had very similar skeletons and considerable diversity in number, were considered as the major active constituents [6], so the development of rapid and economical methods for the identification of these sesquiterpenoid lactones is of great significance. Their preparative separation and purification by conventional methods is tedious, time consuming, with low recoveries and high cost [8,9]. There is no report on the use of HSCCC for the isolation and purification of sesquiterpenoid lactones from Eupatorium lindleyanum DC, we report an efficient method for the preparative isolation and purification of three sesquiterpenoid lactones (structures shown in Figure 1) from Eupatorium lindleyanum DC. by one-step HSCCC
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