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Method for extracting icariin from herba epimedii

A technology of icariin and Huoquancao, which is applied in the field of plant active ingredient extraction, can solve the problems of unstable content and extraction rate, incomplete extraction, cumbersome steps, etc., simplify the process of extraction and separation, and reduce production costs , the effect of improving the extraction rate

Pending Publication Date: 2022-01-28
SHAANXI SCI TECH UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing process of extracting and preparing higher-purity icariin from Epimedium medicinal materials, no matter whether alcohol solution reflux extraction or auxiliary extraction is used, extraction, extraction and separation are required, and each step is cumbersome, incomplete extraction, and loss. Large, unstable content and extraction rate, and use a large amount and variety of organic solvents, the extraction process is complicated, the whole process takes a long time, and the cost is high
The existing process for preparing icariin from Epimedium medicinal material is no longer suitable for the extraction of low-content raw materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0024] Dry the whole herb of Epimedium in the shade, pulverize it with a pulverizer, and pass through an 80-mesh sieve; weigh 40 kg of the whole herb powder of Epimedium in a retort, and add an aqueous solution of sodium carbonate with a pH of 10, which is 1.5% of the weight of the whole herb powder. Float the whole Herb Epimedium loosely, soak for 40 minutes, add water vapor and stir for 60 minutes, filter while hot, put the solid slag in the retort for 60 minutes and stir to extract twice , filtered, combined filtrate, filtrate cooled by ice bath, acidified with concentrated hydrochloric acid to adjust its pH to 4.2, left to settle, filtered to collect precipitate; mother liquor was extracted twice with ethyl acetate at a volume ratio of 1:0.7, and acetic acid was recovered Ethyl, ethyl acetate extracted solids and precipitates were combined to form the crude extract, which was dried at low temperature and weighed 3.28kg. The crude extract was mixed with C18 bonded silica ge...

example 2

[0026] Dry the whole herb of Epimedium in the shade, pulverize it with a pulverizer, and pass through an 80-mesh sieve; weigh 60 kg of the whole herb powder of Epimedium in a retort, and add an aqueous solution of sodium carbonate with a pH of 11, which is 1.4% of the weight of the whole herb powder. Float the whole Herb Epimedium loosely, soak for 30 minutes, add water vapor and stir for 50 minutes, filter while hot, put the solid slag in the retort for 50 minutes and stir to extract twice , filter, combine the filtrate, the filtrate is cooled in an ice bath, acidify with concentrated hydrochloric acid to adjust its pH to 3.5, let it stand for precipitation, and collect the precipitate by filtration; the mother liquor is extracted twice with ethyl acetate at a volume ratio of 1:0.6, and the acetic acid is recovered Ethyl, ethyl acetate extracted solids and precipitates were combined to form the crude extract, which was dried at low temperature and weighed 4.90kg. Mix the crud...

example 3

[0028]Dry the whole herb of Epimedium in the shade, pulverize it with a pulverizer, and pass through an 80-mesh sieve; weigh 80 kg of the whole herb powder of Epimedium in a retort, and add a sodium carbonate aqueous solution with a pH of 10.5, which is 1.48% of the weight of the whole herb powder. Float the whole Herb Epimedium loosely, soak for 35 minutes, add water vapor and stir for 55 minutes, filter while hot, put the solid slag in the retort for 55 minutes and stir to extract twice , filter, and combine the filtrates. The filtrates are cooled in an ice bath, acidified with concentrated hydrochloric acid to adjust their pH to 4.0, left to settle, and filtered to collect the precipitate; the mother liquor is extracted twice with ethyl acetate at a volume ratio of 1:0.6, and the acetic acid is recovered. Ethyl, ethyl acetate extracted solids and precipitates were combined to form the crude extract, which was dried at low temperature and weighed 6.52 kg. Mix the crude extra...

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PUM

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Abstract

The invention provides a method for extracting icariin, the method comprises the following steps: soaking herba epimedii herb powder in 1.4-1.5 times by weight of sodium carbonate aqueous solution with the pH value of 10-11 for about half an hour, introducing water vapor, stirring for about 1 hour, and carrying out hot filtration; introducing water vapor into the solid residues for about 1 hour, stirring, carrying out hot filtration, and repeating the step once; mixing the filtrates, cooling in an ice bath, adjusting the pH value of the filtrate to 3.5-4.2, standing and precipitating, filtering and collecting the precipitate, and drying at low temperature; mixing the dried crude extract with C18 bonded silica gel, carrying out column chromatography, detecting with HPLC during elution, keeping the retention time of a chromatogram of a reference substance for 10.5 min, and intercepting the same component; and distilling and recovering the eluent, and recrystallizing twice. High-purity icariin and other flavonoid substances such as epimedin A, epimedin B and epimedin C can be obtained, the icariin is 0.8 part by weight, the content of the icariin exceeds 98.4%, and the extraction rate exceeds 97.5%.

Description

technical field [0001] The invention belongs to the technical field of extraction of effective plant components, and relates to a method for extracting icariin from whole epimedium herb. Background technique [0002] Icariin (also known as icariin) can enhance the body’s immunity by regulating the balance of T cells, promote the formation and activation of osteoblasts, inhibit osteoporosis, protect cardiomyocytes and increase the number of cardiomyocytes, improve endothelial dysfunction and repair heart disease. Cerebrovascular function, regulating endocrine, antibacterial and anti-inflammatory, anti-oxidation, anti-aging, anti-tumor, enhancing learning and memory, improving reproductive function and other activities, and can also treat Alzheimer's disease, Parkinson, cerebral ischemia, atherosclerosis , rheumatism and other diseases. Icariin is the main active ingredient of Epimedium. In the 2020 edition of Chinese Pharmacopoeia, it is recorded that Epimedium "functions an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H1/08C07H17/07
CPCC07H1/08C07H17/07
Inventor 田光辉刘存芳张必荣张勇陈婷刘洋吴睿刘波张志军
Owner SHAANXI SCI TECH UNIV
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