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Extracting process for epimedium total flavone

A technology of total flavonoids and a new process, which is applied in the field of extracting effective parts of Chinese medicinal materials, can solve the problems of great harm, tediousness, and increased cost, and achieve the effect of overcoming unsafe factors, simple process methods, and environmental protection

Inactive Publication Date: 2006-03-15
吉林省中医中药研究院 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) In Wang Changli's report "Extraction and Separation Process of Epimedium Total Flavonoids" (Chinese Patent Medicine 1996; 18 (5): 1), after comparing the two processes of water and alcohol extraction, the conclusion is that, from industrialization In the analysis of practicability and economic cost of large-scale production, it is believed that the water extraction process is better than the alcohol extraction process, but there is no report on the specific separation and purification method
[0005] (2) Wang Chengjun reported "Research on the Extraction Technology of Epimedium Total Flavonoids" (Journal of Basic Chinese Medicine 2002; 16 (5): 3) which adopted the method of 25 times the amount of 80% ethanol reflux extraction for 1 hour, this method Due to the relatively high concentration of ethanol used, fat-soluble impurities such as chlorophyll may be brought into the extract, which increases the difficulty of subsequent separation and purification, and there are also some disadvantages in terms of practicality and economic cost analysis. The method has not been reported, and the purity of the obtained total flavonoids of Epimedium is unknown
This method is cumbersome, and because ethanol is used to extract and purify methanol, not only the cost increases, but also methanol is harmful to the human body and is not safe.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Get Epimedium medicinal material, add 20 times the amount of water, decoct 3 times, each time for 1 hour, filter, the filtrate is concentrated to a relative density of about 1.05 (50 ° C), add ethanol (to make the alcohol concentration reach 50%), fully Stir, stand for 24 hours, filter, add sodium hydroxide to the filtrate to make the pH value reach 8.5, filter, adjust the filtrate to neutral, recover ethanol, and the residue passes through the pre-treated macroporous adsorption resin D301 column, and elutes with water Until the water eluent is light yellow, use 3 to 4 times (resin bed volume) 70% ethanol for eluting, and recover the ethanol to obtain the total flavonoids. The yield of total flavonoids is 2.5%, and the purity is 72.01%.

Embodiment 2

[0019] Get Epimedium medicinal material, add 25 times the amount of water, decoct 2 times, each time for 1.5 hours, filter, the filtrate is concentrated to a relative density of about 1.04 (55 ° C), add ethanol (to make the alcohol concentration reach 60%), fully Stir, stand for 16 hours, filter, add lime to the filtrate to make the pH value reach 7.5, filter, adjust the filtrate to neutral, recover ethanol, and the residue passes through the pre-treated macroporous adsorption resin D301 column, and is eluted with water to water The eluent was light yellow, and eluted with 3 to 4 times (resin bed volume) 70% ethanol instead, and the ethanol was recovered to obtain the total flavonoids. The yield of total flavonoids is 2.9%, and the purity is 69.80%.

Embodiment 3

[0021] Get the Epimedium medicinal material, add 30 times the amount of water, decoct 2 times, each time for 2 hours, filter, the filtrate is concentrated to a relative density of about 1.05 (50 ° C), add ethanol (to make the alcohol concentration reach 70%), fully Stir, stand for 12 hours, filter, add soda lime to the filtrate, make the pH value reach 8, filter, adjust the filtrate to neutral, recover ethanol, and the residue is eluted with water to The water eluent is light yellow, and it is eluted with 3 to 4 times (resin bed volume) 70% ethanol instead, and the ethanol is recovered to obtain the total flavonoids. The yield of total flavonoids is 2.7%, and the purity is 70.40%.

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PUM

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Abstract

The total epimedium flavone extracting process with medicinal epimedium material includes mixing with water, decoction, filtering, concentrating filtrate, adding ethanol via stirring, settling, filtering, adding alkali or alkali oxide to the filtrate to regulate pH to 7-9, filtering, regulating the filtrate to neutral, recovering ethanol, water elution in processed resin column, ethanol solution elution and recovering ethanol to obtain total epimedium flavone. The said process is low in cost, safe, simple and suitable for industrial production, and the product has purity over 70%.

Description

Technical field: [0001] The invention discloses a new extraction process of total flavonoids of Epimedium, and relates to the technical field of extraction process of effective parts of Chinese medicinal materials. Background technique: [0002] Most of the reports about the extraction and separation methods of flavonoids in Epimedium are the classic method, namely decocting in water (or alcohol extraction), and repeated extraction with ethyl acetate (or n-butanol). Due to the large amount of organic solvent used and the complicated methods, it can only be used in the laboratory, and it is difficult to promote it to production. [0003] In recent years, there are mainly the following reports on the extraction method of total flavonoids from Epimedium. [0004] (1) In Wang Changli's report "Extraction and Separation Process of Epimedium Total Flavonoids" (Chinese Patent Medicine 1996; 18 (5): 1), after comparing the two processes of water and alcohol extraction, the conclusi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07B63/00C07D311/30C07H17/07C07H1/08A61K36/296
Inventor 刘桂荣黄万忠耿琍刘蕾陈岩代兴春
Owner 吉林省中医中药研究院