Preparation of icaritin

A technology of icariin and icariin, which is applied in the field of extracting the active ingredient icariin, can solve the problems of poor deglycolysis efficiency, no use value, and low product yield. Easy to handle, complete desaccharification and high yield

Active Publication Date: 2008-11-12
BEIJING SHENOGEN BIOMEDICAL
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the domestic use of acid hydrolysis, however, hydrochloric acid hydrolysis is easy to form an addition to the double bond on the 8-substituent, resulting in a low yield of the product and no use value, while sulfuric acid hydrolysis can only remove the sugar group at the 7-position , and the sugar group on the 3-position is not easy to hydrolyze, and as a result, only icariin with low sugar group can be obtained. Compared with icariin, its activity is higher, but it is still far from icariin
Patent application (application number 031336353) "Method for preparing low-sugar icariin or aglycon by enzymatically hydrolyzing icariin glycosyl groups", which adopts the fermented enzyme inducer with Epimedium as the strain, and extracts it after fermentation The enzyme used for the sugar hydrolysis of icariin, but the results show that the enzymatic hydrolysis product is a low-sugar, sugar-free, differently substituted icariin or aglycon, indicating that its deglycolysis efficiency is not very good

Method used

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  • Preparation of icaritin
  • Preparation of icaritin
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1. Enzymatic hydrolysis of icariin Add 100g of icariin to 5000ml of 20% ethanol, stir to dissolve, add 10g of β-glucosidase, and hydrolyze at 60°C for 20 hours.

[0033] 2. Post-treatment of the reaction solution: centrifuge the reaction solution and discard the supernatant. The precipitate was dissolved with 2500ml of acetone, the solution was centrifuged, the supernatant was taken out, filtered, the insoluble matter was discarded, and the supernatant was evaporated to dryness.

[0034] 3. Preparation of pure icariin (glycogen):

[0035] Add acetone-water (1:1) 1500ml to recrystallize, place, crystallize, filter and dry to obtain 29g of pure icariin. The purity is over 98% as detected by HPLC. (like figure 1 ) HPLC condition is acetonitrile-1% glacial acetic acid aqueous solution 70:30, detection wavelength 273nm. Melting point: higher than 250°C.

[0036] Overall yield: 53.3%.

Embodiment 2

[0038] 1. Enzymatic hydrolysis of icariin Add 100g of icariin to 5000ml of 20% ethanol, stir to dissolve, add 100g of β-glucosidase, and hydrolyze at 40°C for 30 hours.

[0039] 2. Post-treatment of the reaction solution: centrifuge the reaction solution and discard the supernatant. The precipitate was dissolved with 2500ml of acetone, the solution was centrifuged, the supernatant was taken out, filtered, the insoluble matter was discarded, and the supernatant was evaporated to 25ml per gram (relative to icariin).

[0040] 3 Preparation of pure icariin:

[0041] Take the concentrated supernatant, add an equal amount of water to recrystallize, place, crystallize, filter, and dry to obtain 30.2 g of pure icariin. The purity is over 98% as detected by HPLC. (like figure 2 ) HPLC condition is acetonitrile-1% glacial acetic acid aqueous solution 70:30, detection wavelength 273nm.

[0042] The total yield is 55.5%.

[0043] Because the solvent acetone is used in the aftertreatme...

Embodiment 3

[0045] 3.1 Extraction of total flavonoids from Epimedium

[0046] 3.1.1 Pulverization: Pulverize 10,000 g of dried epimedium and put it into an extraction tank.

[0047] 3.1.2 Extraction: Add 16 times the amount of water to decoct 3 times, 2 hours for the first time, and 1.5 hours for each subsequent time. The three extracts were combined, filtered, and concentrated under reduced pressure to a solution of 0.2 g raw medicinal material / ml.

[0048] 3.1.3 Resin purification: the extract is absorbed by the pre-treated D101 macroporous resin column for total flavonoids (the amount of resin used is about 1.5 times that of medicinal materials.). The flow rate of the extract on the column was 5 column volumes / h. After adsorption, first wash with water until the water eluent is light yellow, about 4 column volumes, and then use 30% ethanol, about 4 column volumes, 50% ethanol, about 4 column volumes, and 90% ethanol after treatment, Wash with water and set aside.

[0049] 3.1.4 Con...

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Abstract

The invention relates to a method for preparing icaritin and is characterized in that: the icaritin is prepared by icariin which is subject to the enzymolysis reaction by beta-glycosidase. The method adopts the beta-glycosidase to perform the enzymolysis reaction for the icariin, the beta-glycosidase has complete deglycolysis and high yield, a self-designed method for extracting the icariin from Herba Epimedii is adopted, the whole technical process has simple and convenient operation, the treatment is convenient after the reaction, and the purity of the product fully meets the pharmaceutical standard.

Description

technical field [0001] The invention relates to the field of traditional Chinese medicines, in particular to a method for extracting icariin, an active ingredient in the traditional Chinese medicine epimedium. Background technique [0002] Epimedium is a commonly used traditional Chinese medicinal material. It is the dry part of the ground of various plants of the genus Epimedium (Epimedium genus) in the Berberidaceae (Berberidaceae). That is, Epimedium brevicornum Maxim), Epimedium sagittatum, Epimedium pubescens, Epimedium wushanenes, Epimedium koreanum Nakai, etc. Epimedium has the functions of invigorating kidney and strengthening yang, strengthening tendons and bones, dispelling wind and dehumidification, and is often used to treat impotence, dripping urine, weak waist and knees, coronary heart disease, chronic bronchitis, neurasthenia and polio. Modern pharmacological studies have proved that Epimedium contains special chemical components and significant biological ac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P17/06C07D311/40C07H1/06C07H1/08
CPCC12P19/605
Inventor 孟坤
Owner BEIJING SHENOGEN BIOMEDICAL
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