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Icaritin preparation method

A technology of icariin and epimedium extract, which is applied in the field of medicine, can solve the problems of low conversion rate of enzymatic hydrolysis and many impurities in the final product, and achieve the effects of improving purity, easy purification, and improving production efficiency

Active Publication Date: 2015-06-17
BEIJING SHENOGEN PHARMA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, in the above three methods, there are defects such as low conversion rate of enzymatic hydrolysis and many impurities in the final product.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 1. Preparation of Epimedium Extract

[0039] 1.1 Extraction

[0040] The present embodiment extracts in stages except the stem, and Epimedium leaves total 490Kg, crush it, and use 14 times, 10 times of amount (v / w) 40% ethanol aqueous solution reflux extraction of 40% volume concentration respectively, 2 times each time Hour. Recover ethanol until the extract has no alcohol smell, and detect the total flavonoids in the extract by high performance liquid chromatography, see attached figure 1 upper half of the picture;

[0041] 1.2 Macroporous resin purification

[0042] Concentrate the ethanol extract obtained in step 1.1 to remove ethanol, and then purify it with a macroporous resin. First, the macroporous resin column was eluted with distilled water having 8 times the volume of the macroporous resin column bed, and the flow rate of distilled water elution was 1 times the column volume / hour. After the elution was completed, the eluent was discarded;

[0043] Wash...

Embodiment 2

[0056] 1. Preparation of icariin by enzymatic hydrolysis

[0057] Weigh 10Kg of the commercially available Epimedium extract, add it into 100L pH=5.5 disodium hydrogen phosphate-citric acid buffer solution, and dissolve it at a stirring speed of 100rpm. When the temperature of the system was kept constant at 57°C, 1.5Kg of β-glucosidase was added to stir the reaction. After 16 hours of constant temperature reaction, the stirring was stopped, and the temperature of the reaction liquid was lowered to 25°C.

[0058] 2. Purification of Icaritin

[0059] After the enzymolysis reaction, the reaction solution was centrifuged, and the filter cake was collected. After drying, the weight was 7.85Kg. After pulverization, 88.11Kg of acetone was added, stirred for 1 hour, filtered, and 64.55Kg of purified water was added to the acetone solution, then heated to 63°C The system solvent was refluxed until the solution was clear. After the solution was slowly cooled to room temperature,...

Embodiment 3

[0061] 1. Preparation of icariin by enzymatic hydrolysis

[0062] Weigh 8.7Kg of the commercially available Epimedium extract, add it into 174L pH=4.8 citric acid-sodium citrate buffer solution, and dissolve it at a stirring speed of 100rpm. When the temperature of the system is kept constant at 45°C, add 0.435Kg of β-glucosidase and stir the reaction. After 20 hours of constant temperature reaction, the stirring was stopped, and the temperature of the reaction liquid was lowered to 30°C.

[0063] 2. Purification of Icaritin

[0064] After the enzymolysis reaction, the reaction solution was centrifuged, and the filter cake was collected. After drying, the weight was 6.55Kg. After crushing, 76.34Kg of acetone was added, stirred for 1 hour, filtered, and 55.93Kg of purified water was added to the acetone solution, and the temperature was raised to 62°C to make the system The solvent was refluxed until the solution was clear. The temperature of the solution was slowly lowe...

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Abstract

The invention provides an icaritin preparation method which comprises the following steps: a, performing the enzymatic hydrolysis reaction of an epimedium extract under the action of Beta-glycosidase; b, filtering an enzymatic hydrolysis reaction product obtained in step a; c, dissolving filter cake obtained after filtration into acetone; and d, adding water to an acetone solution, performing reflux dissolution, keeping the solution standing, performing filtration, and collecting a crystal substance to obtain icaritin. According to the icaritin preparation method, the yield of icaritin is up to 20% relative to the epimedium extract, and the purity of icaritin is up to 99.8%.

Description

technical field [0001] The invention relates to a preparation method of icariin, which belongs to the field of medicine. Background technique [0002] Acradine, also known as icariin and icariin, is a new effective monomer obtained by enzymatic conversion of the epimedium extract extracted from the Chinese herbal medicine Epimedium, and its structure is as follows ( I) Shown: [0003] [0004] The preparation method of the compound is disclosed in CN101302548B. In the method, icariin is used as a raw material, hydrolyzed by β-glucosidase, the precipitate obtained by centrifuging the hydrolyzed product is dissolved in acetone, and the supernatant is obtained by filtering. Then the supernatant was recrystallized with water to obtain pure icariin. [0005] In the Chinese patent that application number is 201010517793.6, disclose a kind of method that adopts naringinase to obtain icariin from icariin, this method dissolves icariin standard substance in ethanol solvent, at ...

Claims

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Application Information

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IPC IPC(8): C12P17/06C07D311/30C07D311/40
Inventor 孟坤汤城徐更袁贤达孔俊琼
Owner BEIJING SHENOGEN PHARMA GRP
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