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Method for quickly separating and preparing natural dihydroflavonoid compounds by using high-speed counter-current chromatography

A high-speed countercurrent chromatography and dihydroflavonoid technology is applied in the field of preparing dihydroflavonoids by a high-speed countercurrent chromatography continuous cycle separation method, which can solve the problems of long time consumption, single compound structure, and difficulty in one-time separation, etc. high purity effect

Active Publication Date: 2018-02-02
FUDAN UNIV
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Problems solved by technology

It has been reported in the literature that flavonoids, such as diosmin, luteolin, and 5,7-dihydroxychromanone, were isolated and purified from peanut shells using conventional HSCCC technology (Niu Dandan et al., Natural Product Research and Development, 2011,23:110-113), but the conventional HSCCC method takes a long time and the structure of the separated compound is relatively single. For Sophora sophora, it is difficult to quickly and simultaneously separate high-purity, complex and similar monomeric flavonoids Compounds

Method used

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  • Method for quickly separating and preparing natural dihydroflavonoid compounds by using high-speed counter-current chromatography
  • Method for quickly separating and preparing natural dihydroflavonoid compounds by using high-speed counter-current chromatography
  • Method for quickly separating and preparing natural dihydroflavonoid compounds by using high-speed counter-current chromatography

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Embodiment 1

[0033] (1) The OptiChrome-300PLUS high-speed countercurrent chromatograph produced by Jiangsu Jiangyin Countercurrent Technology Co., Ltd. was used to improve the separation and purification of samples, and the Agilent 1200HPLC high-performance liquid chromatograph produced by Agilent Co., Ltd. of the United States was used for sample purity analysis;

[0034] Set up a high-speed countercurrent chromatograph, connect the six-way valve a to the back of the instrument detector, connect the six-way valve a to the storage ring, and connect the six-way valve b to the front of the constant flow pump, which is responsible for the switching between the two elution modes of normal elution and cycle elution ( Such as figure 1 shown);

[0035] (2) Preparation of extract samples

[0036] Take the dried root of Sophora japonica, crush it, cold soak and extract it with 95% ethanol three times, combine the extracts, concentrate under reduced pressure, and evaporate to dryness;

[0037] (3)...

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Abstract

The invention belongs to the technical field of medicine, and relates to a method for separating and preparing natural dihydroflavonoid compounds. The method adopts a continuous circulation method ofhigh-speed counter-current chromatography, and a two-phase solvent system which is formed by n-hexane, ethyl acetate, methanol and water is adopted in the high-speed counter-current chromatography toseparate and prepare the dihydroflavonoid compounds from roots of sophora alopecuroide. According to the method, a mode of high-speed counter-current circulating elution, an online storage technique and a reverse elution mode are adopted at the same time, and continuous circulating elution are conducted on flow components which contain the target compound to collect the flow components and obtainflavonoid compounds which comprise sophoratonkin, alopecurone F, lehmannin, alopecurone A, sophora flavanone G and alopecurone B and have the purity of more than 95%; the five dihydroflavonoid compounds and santilin glycoside which have high purity are obtained through one-time separation, the method is simple, convenient and rapid in operation, and no loss of the target compounds is caused by material adsorption during the separation.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a method for separating and preparing natural dihydroflavonoids, in particular to the preparation of dihydroflavonoids by adopting a high-speed countercurrent chromatography (HSCCC) continuous circulation separation method. Background technique [0002] The prior art discloses that Sophora alopecuroides L. is a perennial herb of the genus Sophora in the family Fabaceae, also known as Sophora alopecuroides. It is a commonly used Chinese medicinal material in Northwest my country, and its roots, stems, whole plants and seeds can be used as medicine. Bitter beans are bitter in taste and cold in nature, and have the functions of expelling wind and dampness, clearing heat and detoxification, relieving pain and killing insects. Pharmacological studies have shown that various types of compounds isolated from Sophora Sophora have pharmacological effects such as anti-tumor, immune regulati...

Claims

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Application Information

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IPC IPC(8): C07D311/32C07D311/40C07D493/04C07H17/04C07H1/06
CPCC07D311/32C07D311/40C07D493/04C07H1/06C07H17/04
Inventor 孙仲琳何建明穆青蓝江儿
Owner FUDAN UNIV
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