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Microwave-Assisted Extraction and Purification of Arctiin and Arctigenin from Fructus Arctii by High-Speed Countercurrent Chromatography

Author:
Lü, Haitao, Sun, Zhaoyun, Shan, Hu, Song, Jiying
Source:
Journal of chromatographic science 2016 v.54 no.3 pp. 472-478
ISSN:
1945-239X
Subject:
2,2-diphenyl-1-picrylhydrazyl, Arctium lappa, Fourier transform infrared spectroscopy, acid hydrolysis, antioxidant activity, countercurrent chromatography, free radicals, high performance liquid chromatography, hydrochloric acid, lignans, microwave treatment, nuclear magnetic resonance spectroscopy, solvents
Abstract:
An efficient method for the rapid extraction, separation and purification of bioactive lignans, arctiin and arctigenin, from Fructus arctii by microwave-assisted extraction coupled with high-speed countercurrent chromatography was developed. The optimal extraction conditions of arctiin and arctigenin were evaluated by orthogonal array. Arctigenin could be converted from arctiin by hydrochloric acid hydrolysis. The separations were performed at a preparative scale with two-phase solvents composed of ethyl acetate–ethanol–water (5 : 1 : 5, v/v/v) for arctiin, and n-hexane–ethyl acetate–ethanol–water (4 : 4 : 3 : 4, v/v/v/v) for arctigenin. From 500 mg of crude extract sample, 122.3 mg of arctiin and 45.7 mg of arctigenin were obtained with the purity of 98.46 and 96.57%, and the recovery of 94.3 and 81.6%, respectively. Their structures were determined by comparison with the high-performance liquid chromatography retention time of standard substance as well as UV, FT-IR, electrospray ion source (ESI)–MS, ¹H-NMR and ¹³C-NMR spectrum. According to the antioxidant activity assay, arctigenin had stronger 1,1-diphenyl-2-picrylhydrazyl free radicals scavenging activity.
Agid:
6260910