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Method for preparing high-purity luteolin

A technology for the separation and purification of luteolin, which is applied in the field of extraction and separation of natural compounds, can solve the problems of complex operation steps, complex operation equipment, and long production cycle, and achieve the effects of simplifying processing steps, saving operating time, and reducing the degree of danger

Active Publication Date: 2018-11-23
昌邑市银江生物科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] All of the above methods can give luteolin with a certain purity, but some processes have complex operation steps, long production cycle, and complex operating equipment, etc., which are difficult to apply to industrial scale production, high cost, and complicated operation.
[0006] The chelation phenomenon of flavonoids and metal ions is frequently reported

Method used

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  • Method for preparing high-purity luteolin
  • Method for preparing high-purity luteolin
  • Method for preparing high-purity luteolin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A. In the peanut shell extract of 70% ethanol water of 100mL, directly add the ferric chloride aqueous solution of 40mg / mL, add the ferric chloride aqueous solution amount and guarantee that the mol ratio of metal ion and luteolin is 1 / 3, after adding , Chelation reaction time is 2hr. The temperature of the chelation reaction is 30°C; the precipitate generated by the chelation reaction is separated by filtration;

[0025] B. Dissolving the above precipitate with a hydrochloric acid solution of pH=4 for 20 minutes;

[0026] C. add 5% EDTA solution in above-mentioned acid solution, the volume ratio of EDTA solution and above-mentioned acid solution is 1 / 2. After fully mixing, the solution was evaporated to dryness, and the precipitate was dissolved with 10 times the amount of methanol, and the filtrate was concentrated and evaporated to dryness to obtain crude luteolin, which was recrystallized with 50% ethanol aqueous solution, and the purity reached 95%.

Embodiment 2

[0028] A. In the peanut shell extract of 70% ethanol water of 100mL, directly add the ferric chloride aqueous solution of 20mg / mL, add the ferric chloride aqueous solution amount and ensure that the mol ratio of metal ion and luteolin is 1 / 3, after adding , Chelation reaction time is 2hr. The temperature of the chelation reaction is 30°C; the precipitate generated by the chelation reaction is separated by filtration;

[0029] B. Dissolving the above precipitate with a hydrochloric acid solution of pH=6 for 20 minutes;

[0030] C. add 5% EDTA solution in above-mentioned acid solution, the volume ratio of EDTA solution and above-mentioned acid solution is 1 / 1. After fully mixing, the solution was evaporated to dryness, and the precipitate was dissolved with 10 times the amount of methanol, and the filtrate was concentrated and evaporated to dryness to obtain crude luteolin, which was recrystallized with 50% ethanol aqueous solution, and the purity reached 92%.

Embodiment 3

[0032] A. In the peanut shell extract of 70% ethanol water of 100mL, directly add the ferric chloride aqueous solution of 60mg / mL, add the ferric chloride aqueous solution amount to ensure that the mol ratio of metal ion and luteolin is 1 / 2, after adding , Chelation reaction time is 5hr. The temperature of the chelation reaction is 60°C; the precipitate generated by the chelation reaction is separated by filtration;

[0033] B. Dissolving the above precipitate with a hydrochloric acid solution of pH=2 for 20 minutes;

[0034] C. add 5% EDTA solution in above-mentioned acid solution, the volume ratio of EDTA solution and above-mentioned acid solution is 1 / 1. After fully mixing, the solution was evaporated to dryness, and the precipitate was dissolved with 10 times the amount of methanol, and the filtrate was concentrated and evaporated to dryness to obtain crude luteolin, which was recrystallized with 50% ethanol aqueous solution and had a purity of 94%.

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Abstract

The invention discloses a method for preparing high-purity luteolin. According to the method, a ferric ion solution and a peanut shell extracting solution are utilized for being mixed, a ferric ion and flavonoid chelation principle is utilized, and flaconoid of luteolin and the like are separated and purified from the extracting solution. The method is characterized in that the ferric iron salt solution is directly added into the peanut shell extracting solution, and chelate is prepared from ferric ion and flavonoid of luteolin and the like in extractive. After chelate precipitate is separatedand dissolved, EDTA and iron are chelated, luteolin is dissociated out, and the high-purity luteolin is obtained through ethyl alcohol water recrystallization. The method disclosed by the invention has the advantages of simple and convenient purifying process, low use cost, no toxic reagent and low energy consumption; thus, the method is a simple, convenient, green and high-efficiency technology.

Description

technical field [0001] The invention relates to a method for separating and purifying flavonoids such as luteolin from the extract by mixing ferric ion solution with peanut shell extract and using the principle of iron ion and flavonoid chelation. It belongs to the field of natural compound extraction and separation. Background technique [0002] In the 1960s, scientists extracted flavonoids from Ginkgo biloba and used them clinically. Flavonoids have also been recognized worldwide as natural compounds. Ginkgo biloba extracts have also become one of the most consumed plant extracts in the world. Flavonoids are widely found in the roots, stems, and leaves of certain plants in nature, with a total of more than 4,000 species. The efficacy of flavonoids is multifaceted, and the efficacy of flavones with different molecular structures is also very different. It is generally believed that flavones are a strong antioxidant that can effectively remove oxygen free radicals in the bo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/30C07D311/40
CPCC07D311/30C07D311/40
Inventor 孙立权李林强姜亚丽赵峰强
Owner 昌邑市银江生物科技有限公司