Method for preparing and separating tectorigenin from iris in high-speed countercurrent chromatography by one step

Abstract

The invention relates to a method for separating and purifying monomeric compound of tectorigenin from iris, in particular to a method for separating and purifying tectorigenin from iris. The method comprises the following steps: dipping with methanol solution to extract and prepare iris coarse extracts, adding a little of water in the coarse extracts to dilute, extracting with ethyl acetate solution and removing water soluble foreign matters, concentrating the ethyl acetate into an extract, separating and purifying an ethyl acetate sample in a high-speed countercurrent chromatography by one step to prepare the tectorigenin with purity higher than 95%. The method has simple operation, high separation efficiency and high purity of products and is suitable for the industrial production.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a method for separating and purifying irisinin from iris by high-speed countercurrent chromatography. Background technique [0002] Iris (Sichuan Shegan) is the dried rhizome of Iris tectorum Maxim, a plant of the family Iridaceae. It has the effects of clearing away heat and detoxifying, eliminating phlegm and relieving sore throat. It is mainly used for sore throat, phlegm, cough and asthma. Department of recorded varieties (National Pharmacopoeia Committee. Pharmacopoeia of the People's Republic of China [S], one, Beijing: Chemical Industry Press. 2005: 28-29.). Mainly produced in Sichuan, Chongqing, Guizhou, Yunnan, Guangxi and other provinces. Modern studies have found that iris is rich in isoflavones, of which irisin is the main active ingredient in iris (Shang logistics, Qin Minjian, Wu Jinrong. Chemical constituents of iris [J]. China Natural Medicine, 2007, 5 (4): 312...

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Problems solved by technology

[0004] At present, traditional methods such as column chromatography are used at home and abroad to separate and purify irisinin in Iris (Yuan Chongjun, Wang Jia, Chen Shuai, etc. Research on the chemical components of Iris [J]. Natural Product Research and Development, 2008, 20( 9): 444-446, 449; Qiu Qinghao, Zhang Zhiguo, Wang Jianhua, etc. Research on the chemical constituents of isoflavones in Iris [J], Chinese Materia Medica, 2009, 32(9): 1392-1394.), this kind of method is often used A large amount of toxic organic solvents such as chloroform and methanol will cause environmental pollution, and the shortcomings of column chromatography are long separation cycle, low recovery rate and unsatisfactory separation effect

Recently, Fan Guorong et al. (Fan Guorong, Zhou Tingting, Feng Chao, Xie Ying, Wen Jun, Cui Lijun, Chen Danxia, ​​Li Ji, Xie Rui, Wei Hua, Zhang He. A method for the separation of isoflavone monomer compounds in Shegan by secondary high-speed countercurrent chromatography , Publication No.: CN101357933A, Publication Date: February 4th, 2009) Utilize HSCCC to separate and obtain irisinin from different genus plants of the same family of Iris (Belamcandachinensis (L.) DC.), the method used is loaded down with trivial details, takes a long time

In the existing literature, there is no report that HSCCC is used for one-step rapid preparation and isolation of irisin in iris

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