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Method for separating and purifying effective ingredients from fine felt hairy honeysuckle

A technology for separation and purification of hydroxyl, applied in the field of separation and purification of active ingredients in Lonicera velvet, to achieve the effects of improving utilization, saving separation and purification costs, and saving reagent consumption

Inactive Publication Date: 2013-02-13
CHENGDU UNIV OF TRADITIONAL CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there are no related reports on the separation and purification of 5-hydroxy-7,3',4'-trimethoxyflavone and other compounds from Lonicera velvet

Method used

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  • Method for separating and purifying effective ingredients from fine felt hairy honeysuckle
  • Method for separating and purifying effective ingredients from fine felt hairy honeysuckle
  • Method for separating and purifying effective ingredients from fine felt hairy honeysuckle

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Example 1 Separation and purification method of 5-hydroxy-7,3',4'-trimethoxyflavone

[0064] (1) Weigh 1.9Kg of dried flower buds of Lonicera similes Hemsl, reflux extract with 90%, 80%, 70% ethanol, the material ratio is 1:8, filter, recover ethanol under reduced pressure, and obtain extract. After determination, the extract contains 3.39% of total flavonoids.

[0065] (2) Take the above extract, add water to prepare the upper column solution, the concentration of the upper column solution is 0.10g / ml in terms of crude drug, put it on the macroporous adsorption resin column, and use water in turn, the concentration is 10%, 20%, 40%, 60% , 80%, 95% V / V ethanol elution, collect 95% ethanol part;

[0066] (3) Take the obtained ethanol fraction, recover the solvent, and perform silica gel column chromatography (200-300 mesh, 350g, column volume 925ml), use cyclohexane-ethyl acetate=20:1~0:1, ethyl acetate -Methanol=5:1~0:1 system for gradient elution, each fraction is 15...

Embodiment 2

[0085] The separation and purification method of embodiment 2 β-sitosterol

[0086] (1) Weigh 475g of dried flower buds of Lonicera similes Hemsl, extract with 90%, 80%, and 70% ethanol under reflux, the material ratio is 1:8, filter, recover ethanol under reduced pressure, and obtain 95g of extract, (That is, 1g of extract is equivalent to 5g of crude drug). After determination, the extract contains 3.39% of total flavonoids.

[0087] (2) Take the above extract, add water to prepare the upper column solution, the concentration of the upper column solution is 0.10g / ml in terms of crude drug, put it on the macroporous adsorption resin column, and use water in turn, the concentration is 10%, 20%, 40%, 60% , 80%, 95% V / V ethanol elution, collect 95% ethanol part;

[0088](3) Take the obtained ethanol part, recover the solvent, and perform silica gel column chromatography (200-300 mesh, 350g), use cyclohexane-ethyl acetate=20:1~0:1, ethyl acetate-methanol=5 : 1~0:1 system for g...

Embodiment 3

[0095] Example 3 The separation and purification method of β-carotin

[0096] (1) Weigh 475g of dried flower buds of Lonicera similes Hemsl, extract with 90%, 80%, and 70% ethanol under reflux, the material ratio is 1:8, filter, recover ethanol under reduced pressure, and obtain 95g of extract, (That is, 1g of extract is equivalent to 5g of crude drug). After determination, the extract contains 3.39% of total flavonoids.

[0097] (2) Take the above extract, add water to prepare the upper column solution, the concentration of the upper column solution is 0.10g / ml in terms of crude drug, put it on the macroporous adsorption resin column, and use water in turn, the concentration is 10%, 20%, 40%, 60% , 80%, 95% V / V ethanol elution, collect 95% ethanol part;

[0098] (3) Take the obtained ethanol part, recover the solvent, and perform silica gel column chromatography (200-300 mesh, 350g), use cyclohexane-ethyl acetate=20:1~0:1, ethyl acetate-methanol=5 : 1~0:1 system for gradie...

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Abstract

The invention discloses a method for separating and purifying 5-hydroxy-7, 3', 4'-triethoxy flavone, beta-sitosterol or / and betal-daucosterol from fine felt hairy honeysuckle. According to the method for separating and purifying 5-hydroxy-7, 3', 4'-triethoxy flavone, beta-sitosterol or / and betal-daucosterol from fine felt hairy honeysuckle, disclosed by the invention, the purity of each obtained compound is high, the new use value of fine felt hairy honeysuckle is developed, and the definition of pharmacodynamic material of fine felt hairy honeysuckle is favorable.

Description

technical field [0001] The invention relates to a method for separating and purifying active ingredients in Lonicerae pilosula, and mainly relates to a method for separating and purifying 5-hydroxy-7,3',4'-trimethoxyflavone, β-sitosterol and β-carotin. Background technique [0002] Lonicera similes Hemsl is the mainstream variety of honeysuckle produced in Sichuan. It is widely distributed and has a large resource reserve. According to the survey, the honeysuckle distributed in the professional market of Chinese medicinal materials in Hehuachi, Chengdu, and the honeysuckle used by traditional Chinese medicine stores and medical institutions in Sichuan Province are mostly Nanjiang produces honeysuckle (Lonicera chinensis) and sells it to all parts of the country. At present, 22 honeysuckle professional demonstration villages have been built in Nanjiang County, Sichuan Province. The total planting area of ​​honeysuckle in the county has reached 260,000 mu, and honeysuckle tome...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/30C07D311/40C07J9/00C07J17/00
Inventor 马逾英郑光雅卢晓琳穆向荣
Owner CHENGDU UNIV OF TRADITIONAL CHINESE MEDICINE
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