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超临界二氧化碳萃取虎杖中的大黄素和大黄素甲醚并随后通过半制备色谱法进行分离。

Supercritical CO2 extraction of emodin and physcion from Polygonum cuspidatum and subsequent isolation by semipreparative chromatography.

作者信息

Lu Hong-Mei, Ni Wang-Dong, Liang Yi-Zeng, Man Rui-Lin

机构信息

College of Chemistry and Chemical Engineering, Central South University, Changsha, PR China.

出版信息

J Sep Sci. 2006 Sep;29(14):2136-42. doi: 10.1002/jssc.200600012.

Abstract

Emodin and physcion are abundant anthraquinone compounds found in the traditional Chinese medicinal herb Polygonum cuspidatum Sied. et Zucc. In this paper, emodin and physcion were successfully extracted with supercritical CO2 plus ethanol modifier after the extraction conditions were optimized with uniform design-sequential optimization. Results showed that the ethanol modifier concentration was the main factor for the effective extraction of the emodin. The optimal extraction condition was obtained: 20 MPa, 30 degrees C, and 95% ethanol, at which the yields of emodin and physcion were 0.616 and 0.178 g/100 g, respectively. The yield obtained by supercritical fluid extraction (SFE) was a little lower than that obtained by sonication extraction (SE). The crude extract obtained by SFE was further isolated and purified by semipreparative chromatography with the mobile phase composed of methanol-water (90:1, v/v). Emodin and physcion were obtained with purity 98.6 and 99.1%, respectively, when determined by HPLC, and identification was performed by retention time and UV spectra of the standards. The result suggested that SFE is an alternative and promising method for extraction of the two compounds from P. cuspidatum owing to its environment-friendly properties and fewer coextracts.

摘要

大黄素和大黄素甲醚是传统中药虎杖中含量丰富的蒽醌类化合物。本文采用均匀设计-序贯优化法对提取条件进行优化后,成功地用超临界CO₂加乙醇改性剂提取了大黄素和大黄素甲醚。结果表明,乙醇改性剂浓度是大黄素有效提取的主要因素。得到最佳提取条件为:20MPa、30℃和95%乙醇,此时大黄素和大黄素甲醚的得率分别为0.616和0.178g/100g。超临界流体萃取(SFE)得到的得率略低于超声提取(SE)。SFE得到的粗提物通过半制备色谱进一步分离纯化,流动相为甲醇-水(90:1,v/v)。通过HPLC测定,大黄素和大黄素甲醚的纯度分别为98.6%和99.1%,并通过标准品的保留时间和紫外光谱进行鉴定。结果表明,由于SFE具有环境友好和共提取物较少的特点,是从虎杖中提取这两种化合物的一种有前途的替代方法。

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