Xiao-Dan Hu1, Ai-Dong Sun, De-Quan Zhang. 1. College of Biological Sciences and Biotechnology, Beijing Forestry University, Beijing 100083, China. huxiaodan2008@sina.com.cn
Abstract
OBJECTIVE: To develop an efficient method for the separation of anthocyanins from Perilla frutescens. METHODS: Freeze-dried Perilla frutescens was extracted with 1% HCl. After purified by Amberlite XAD-7 column chromatography, the bioactive anthocyanins were separated by high-speed countercurrent chromatography (HSCCC). The structures of the compounds were elucidated by 1H- and 13C-NMR spectroscopy. RESULTS: When the HSCCC separation was performed with a two-phase solvent system composed of n-butanol-tert-butyl methyl ether-acentonitrile-water (2:2:1:5 + 0.1% TFA) by eluting the mobile phase at a flow rate of 3.0 mL/min and a revolution speed of 800 r/min, 10.1 mg malonylshisonin and 8.6 mg shisonin were obtained from 1.0 g of the XAD-7 extract. The purities of malonylshisonin and shisonin were 96.7% and 97.5%, respectively. CONCLUSION: HSCCC is a fast and efficient technique to prepare pure malonylshisonin and shisonin from Perilla frutescens.
OBJECTIVE: To develop an efficient method for the separation of anthocyanins from Perilla frutescens. METHODS: Freeze-dried Perilla frutescens was extracted with 1% HCl. After purified by Amberlite XAD-7 column chromatography, the bioactive anthocyanins were separated by high-speed countercurrent chromatography (HSCCC). The structures of the compounds were elucidated by 1H- and 13C-NMR spectroscopy. RESULTS: When the HSCCC separation was performed with a two-phase solvent system composed of n-butanol-tert-butyl methyl ether-acentonitrile-water (2:2:1:5 + 0.1% TFA) by eluting the mobile phase at a flow rate of 3.0 mL/min and a revolution speed of 800 r/min, 10.1 mg malonylshisonin and 8.6 mg shisonin were obtained from 1.0 g of the XAD-7 extract. The purities of malonylshisonin and shisonin were 96.7% and 97.5%, respectively. CONCLUSION:HSCCC is a fast and efficient technique to prepare pure malonylshisonin and shisonin from Perilla frutescens.