Method for separating isoflavones monomeric compound in blackberry lily by high speed countercurrent chromatography

A high-speed countercurrent chromatography and compound technology, which is applied in the field of separation and purification of high-purity monomer compound irisin, to achieve high separation efficiency, effective extraction, simple and fast method

Inactive Publication Date: 2009-02-04
SECOND MILITARY MEDICAL UNIV OF THE PEOPLES LIBERATION ARMY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] At home and abroad, there is no application of high-speed countercurrent chromatography technology to the separation and purification of monomeric compounds in Shegan, a traditional Chinese medicine.

Method used

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  • Method for separating isoflavones monomeric compound in blackberry lily by high speed countercurrent chromatography
  • Method for separating isoflavones monomeric compound in blackberry lily by high speed countercurrent chromatography
  • Method for separating isoflavones monomeric compound in blackberry lily by high speed countercurrent chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] 1. Preparation of Shegan crude extract:

[0047] Take 20 g of dry powdered medicinal materials, ultrasonically extract 2 times with 10 times the amount of 70% ethanol aqueous solution, each time for 30 minutes, filter and combine the filtrates, evaporate the organic phase under reduced pressure in a water bath at 60°C, and dry in vacuo to obtain a crude extract of 3.05 g. g, yield 15.3%.

[0048] 2. Separation and preparation by high-speed countercurrent chromatography:

[0049] High-speed countercurrent chromatography (Shenzhen Tongtian Biochemical Co., Ltd.) was used to separate and purify irisin, irisin, irisin, irisaxanthin and subirisanthin.

[0050] A. The two-phase solvent system of the primary high-speed countercurrent chromatography is n-hexane: n-butanol: methanol: water = 1:4:1.5:6. After fully shaking in the separatory funnel, the layers were statically separated, the upper phase was the stationary phase, and the lower phase was the mobile phase. First ma...

Embodiment 2

[0059] 1. Preparation of Shegan crude extract:

[0060] The preparation of the dry crude extract is the same as in Example 1.

[0061] 2. Separation and preparation by high-speed countercurrent chromatography:

[0062] High-speed countercurrent chromatography (Shenzhen Tongtian Biochemical Co., Ltd.) was used to separate and purify irisin, irisin, irisin, irisaxanthin and subirisanthin.

[0063] A. Preparation of iridin and iridin by high-speed countercurrent separation

[0064] Using four consecutive injections, each injection volume is 200mg, each time saves the balance time before the injection and the time before the peak after the injection is nearly 4 hours, the solvent system of the stationary phase and the mobile phase under the high-speed countercurrent condition is n-hexane:n-butanol:methanol:water=1:4:1.5:6. The high-speed countercurrent separation preparation method and steps of iridin and iridin are the same as in Example 1. Samples were injected at time 0 min...

Embodiment 3

[0067] 1. Preparation of Shegan crude extract:

[0068] Take 20g of dried and dried medicinal material coarse powder, and use 8 times the amount of anhydrous ethanol aqueous solution for microwave-assisted extraction once, microwave power 800w, temperature 70°C, extraction time 10 minutes, filter, the filtrate is evaporated to dryness under reduced pressure in a water bath at 60°C, vacuum After drying, 2.89 g of the crude extract was obtained, with a yield of 14.5%.

[0069] 2. Separation and preparation by high-speed countercurrent chromatography:

[0070] High-speed countercurrent chromatography (Shenzhen Tongtian Biochemical Co., Ltd.) was used to separate and purify irisin, irisin, irisin, irisaxanthin and subirisanthin.

[0071] A. Preparation of iridin and iridin by high-speed countercurrent separation

[0072] The two-phase solvent system of the primary high-speed countercurrent chromatography is ethyl acetate:n-butanol:water=2:1:3. The methods and steps for the sepa...

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Abstract

The invention relates to the medical technical field, in particular to a method for separating and purifying individual compounds of tectoridin, wild tectoridin, tectorigenin, wild tectorigenin and sub wild tectorigenin from blackberry lily. The column chromatography, recrystallization, and the like, are mostly adopted at home and abroad to separate and purify effective monomers in the blackberry lily. The methods have the problems of high cost, complex operation, serious sample loss, etc. The invention adopts secondary high-speed countercurrent chromatography to separate the individual compounds in the blackberry lily, and particularly the technology of the secondary high-speed countercurrent chromatography with two sets of different solvent systems is adopted to separate target compounds of tectoridin, wild tectoridin, tectorigenin, wild tectorigenin and sub wild tectorigenin from other interference components with similar polarity, thus obtaining target compounds with high purity. The method is simple in operation, high in separation efficiency and good in product purity, and sample can be continuously introduced so that the method is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a method for separating and purifying high-purity monomeric compounds irisin, irisin, irisin, irisaxanthin and subirisanthin from iridaceae shegan. Background technique [0002] Shegan is the dried rhizome of Belamcanda Chinesis (L.) DC., a plant of the family Iridaceae. It has the effects of detoxifying the throat, clearing the lungs and eliminating phlegm. It is mainly produced in Hubei, Henan, Jiangsu, Anhui, Hunan, Zhejiang, Guizhou, It is also produced in Yunnan and other places. In a few areas of Guangdong and Guangxi, the whole herb is dried with Shegan. Shegan was first recorded in "Shen Nong's Materia Medica". Pharmacological and clinical experiments have shown that isoflavones in Shegan have significant anti-inflammatory, antibacterial, antiviral, free radical scavenging, anti-allergic and other biological activities and pharmacological effects. Among them, Tectoridin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07D311/36A61K36/88
Inventor 范国荣周婷婷冯超谢瑛闻俊崔莉俊陈丹霞李霁解蕊魏华张鹤
Owner SECOND MILITARY MEDICAL UNIV OF THE PEOPLES LIBERATION ARMY
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