Application of preparative high-speed counter-current chromatography for separation and purification of arctiin from...

Following an initial clean-up step on the AB-8 resin (polystyrene resin, 0.3-1.25 mm: 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 159 mg of arctiin at 98% purity was obtained from 350 mg of the crude extract (containing 49% arctiin) with 91% recovery. The preparative isolation and purification of arctiin by HSCCC was completed in 5 h 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).