高速逆流色谱法从紫苏中分离花青素

Separation of anthocyanins from Perilla frutescens by high speed countercurrent chromatography.

作者信息

Hu Xiao-Dan, Sun Ai-Dong, Zhang De-Quan

机构信息

College of Biological Sciences and Biotechnology, Beijing Forestry University, Beijing 100083, China.

出版信息

Zhong Yao Cai. 2010 Oct;33(10):1586-8.

PMID:21351722

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.

摘要

目的

开发一种从紫苏中分离花青素的高效方法。

方法

用1%盐酸提取冻干的紫苏。经Amberlite XAD - 7柱色谱纯化后，通过高速逆流色谱（HSCCC）分离生物活性花青素。通过¹H - 和¹³C - NMR光谱鉴定化合物的结构。

结果

当使用由正丁醇 - 叔丁基甲基醚 - 乙腈 - 水（2:2:1:5 + 0.1%三氟乙酸）组成的两相溶剂系统进行HSCCC分离时，以3.0 mL/min的流速和800 r/min的转速洗脱流动相，从1.0 g XAD - 7提取物中获得了10.1 mg丙二酰矢车菊素和8.6 mg矢车菊素。丙二酰矢车菊素和矢车菊素的纯度分别为96.7%和97.5%。