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Method for extracting and separating high-purity amentoflavone from selaginella plant

A technology of abiflavonoids from Selaginella spica and Selaginella, which is applied in the field of separation and purification of high-purity abiflavones from Selaginella spiconiae, which can solve the problems of cumbersome extraction process of total flavonoids from Selaginella

Active Publication Date: 2019-03-01
CHINA PHARM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method obtains the total flavonoids extract of Selaginella chinensis, and the process is loaded down with trivial details, and uses flammable and explosive organic solvent

Method used

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  • Method for extracting and separating high-purity amentoflavone from selaginella plant
  • Method for extracting and separating high-purity amentoflavone from selaginella plant
  • Method for extracting and separating high-purity amentoflavone from selaginella plant

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Embodiment 2

[0030] Example 2: Research on the Ethanol-pH Gradient Elution Process of Macroporous Adsorption Resin

[0031]The conventional macroporous adsorption resin column chromatography process, gradient elution with aqueous ethanol, and 40% (v / v) ethanol elution can effectively remove the water-soluble impurities in the sample solution, but the leakage of the target compound afiflavone is relatively serious; further When 70% (v / v) ethanol is used for elution, the target compound, biflavone, can be eluted, and the elution is 8 column volumes, and the process transfer rate is about 60%. The residue of amiflavone in the resin column is relatively serious; increasing the concentration of ethanol to elute the pure segment can improve the transfer rate of the process, but the impurities cannot be effectively separated. HPD-100 macroporous adsorption resin has a strong adsorption capacity for biflavonoids under weak acidic pH conditions, and a strong desorption capacity for flavonoids under...

Embodiment 3

[0051] 1. Medicinal material extraction: crush the medicinal material of Selaginella chinensis into 20 meshes, take 1Kg, add 10 times the weight of 85% (v / v) ethanol to reflux and extract twice, each time for 1 hour, filter, combine the two extracts and recover under reduced pressure solvent to obtain the concentrated solution of medicinal material alcohol extraction, containing 13.5 g of amiflavone.

[0052] 2. Macroporous adsorption resin column chromatography: extract the concentrated solution of medicinal materials with alcohol, filter, and load the filtrate on HPD-100 macroporous adsorption resin column, pH 5, 40% (v / v) ethanol aqueous solution for 3 column volumes , and then use pH 7, 70% (v / v) ethanol aqueous solution to elute 4 column volumes, combine the fractions of 4 column volumes eluted with 70% (v / v) ethanol aqueous solution, and recover the solvent under reduced pressure to dryness to obtain 14.7g of the enriched part of the amiflavones of Suifa chinensis is 70....

Embodiment 4

[0056] 1. Medicinal material extraction: crush Selaginella chinensis into 20 meshes, take 1Kg, add 8 times the weight of 95% (v / v) ethanol to reflux and extract twice, each time for 1 hour, filter, combine the two extracts and recover under reduced pressure solvent, to obtain the medicinal material alcohol extraction concentrate, containing 6.98g of amiflavone.

[0057] 2. Macroporous adsorption resin column chromatography: extract the concentrated solution of medicinal materials with alcohol, filter, and load the filtrate on HPD-100 macroporous adsorption resin column, pH 5, 40% (v / v) ethanol aqueous solution for 3 column volumes , then use pH 7, 70% (v / v) aqueous ethanol to elute 4 column volumes, combine the fractions of 4 column volumes eluted with 70% (v / v) ethanol aqueous solution, reclaim the solvent under reduced pressure to dryness, and obtain 7.1 g of the enriched part of the amiflavones of Suifa chinensis is 69.8%.

[0058] 3. Methanol recrystallization: add the me...

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Abstract

The invention discloses a method for extracting and separating high-purity amentoflavone from a selaginella plant. The method comprises the following steps: separating an amentoflavone crude product from a selaginella plant alcohol extract by taking non-polar macro-porous resin as a separation material with a hydrous ethanol-pH gradient elution process; and separating to obtain the high-purity amentoflavone through the processes of alkaline methanol dissolving acidic precipitation and ethanol recrystallization. The amentoflavone is 98 percent or above in content, and is 50 percent or above inprocess transfer rate.

Description

technical field [0001] The invention belongs to the technical field of traditional Chinese medicines, and in particular relates to a method for separating and purifying high-purity amiflavonoids from Selaginella genus. Background technique [0002] Amentoflavone, also known as Amentoflavone, widely exists in Selaginella plants. Pharmacological studies have shown that the biflavones of Suicha chinensis have pharmacological activities such as anti-inflammation, anti-virus, anti-cancer, hypoglycemic and neuroprotective. The development and application of biflavonoids from Spinica spiconiae as medicinal raw materials has important research value. Selaginella S. tamariscina and Jiangnan Selaginella S. moellendorffii contain a large amount of biflavonoids (0.4-1.4%), and the structural analogues are relatively complex. Research and development of an industrialized preparation and isolation from Selaginella plants The preparation process of high-purity medicinal raw material Bifl...

Claims

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Application Information

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IPC IPC(8): C07D311/30C07D311/40
CPCC07D311/30C07D311/40
Inventor 汪豪马海燕陈骁赵盼盼叶文才
Owner CHINA PHARM UNIV
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