Application of preparative high-speed counter-current chromatography for separation and purification of arctiin from Fructus Arctii
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文摘
Following an initial clean-up step on the AB-8 resin (polystyrene resin, 0.3–1.25mm: NanKai Chemical Factory, Tianjin, China), high-speed counter-current chromatography (HSCCC) was used to purify an arctiin from an extract of the fruits of the Arctium lappa L. Arctiin is a major lignan compound in the traditional Chinese medicinal herb A. lappa L. The two-phase solvent system used was composed of ethyl acetate–n-butanol–ethanol–water at an optimized volume ratio of 5:0.5:1:5 (v/v/v/v). The upper phase was used as the mobile phase in the head to tail elution mode. A total amount of 159mg of arctiin at 98 % purity was obtained from 350mg of the crude extract (containing 49 % arctiin) with 91 % recovery. The preparative isolation and purification of arctiin by HSCCC was completed in 5h in a separation. Identification of the target compound was performed by LC–electrospray ionization MS and 13C-NMR. The structure of the product was further confirmed by comparison with authentic sample (National Institute of the Control of Pharmaceutical and Biological Products, Beijing, China).