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Method for preparing hydrated icaritin

A technology for hydrating icariin and icariin, which is applied in fermentation and other directions, can solve the problems of low content and achieve high yield and convenient processing

Active Publication Date: 2010-12-15
BEIJING SHENOGEN BIOMEDICAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because of its low content in plants, it cannot be prepared industrially (Chemical and pharmacological investigations of Epimedium species: a survey, Prog.Drug Res. 2003;60,1-57

Method used

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  • Method for preparing hydrated icaritin
  • Method for preparing hydrated icaritin
  • Method for preparing hydrated icaritin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1.1 Reaction of icariin with hydrochloric acid solution:

[0028] Take 5 g of icariin (content above 90%), add it to 250 mL of 3N hydrochloric acid solution (concentrated hydrochloric acid and water are prepared at a volume ratio of 3:7), stir, gradually raise the temperature to 80 ° C, and maintain it for 1 hour. After the reaction is over, cool and place to make the precipitation complete. Filter, and wash the precipitate with water several times to neutrality (if it cannot be washed to neutrality, a small amount of NaOH solution can be used to neutralize the acidity). The filtrate was discarded or kept for the next reaction.

[0029] 1.2 Reaction of hydrochloric acid reaction product with cellulase

[0030] Add the above hydrochloric acid reaction product to 250mLNaH 2 PO 4 -Na 2 HPO 4 (pH 5.0, 50 uM) buffer solution, then add about 5 mL of cellulase (comprehensive enzyme activity ≥ 18,000 u / mL), and stir at 40°C for 36 hours. After the reaction, cool down, ad...

Embodiment 2

[0048] 2.1 The reaction between icariin and cellulase

[0049] Take icariin 5g (content above 90%), add to 250mLNaH 2 PO 4 -Na 2 HPO 4 (pH 4.8, 50 uM) buffer solution, then add about 5 mL of cellulase (comprehensive enzyme activity ≥ 18,000 u / mL), and stir at 50°C for 24 hours. After the reaction is over, cool and place to make the precipitation complete. Filter and wash the precipitate with water several times.

[0050] 2.2 Reaction of enzymatic hydrolysis product with hydrochloric acid solution:

[0051] The above enzymatic hydrolysis product was added to 500 mL of 1N hydrochloric acid solution (concentrated hydrochloric acid and water were prepared at a volume ratio of 1:10), stirred, and the temperature was gradually raised to 60° C. and maintained for 8 hours. After the reaction is over, cool and place to make the precipitation complete and filter. The precipitate was washed with water until neutral.

[0052] 2.3 Aftertreatment of the reaction solution: (same as E...

Embodiment 3

[0055] 3.1 Reaction of icariin with hydrochloric acid solution:

[0056] Take 5 g of icariin (content above 90%), add it to 500 mL of 1N hydrochloric acid solution (concentrated hydrochloric acid and water are prepared at a volume ratio of 1:10), stir, gradually raise the temperature to 80 ° C, and maintain it for 8 hours. After the reaction is over, cool and place to make the precipitation complete. Filter, and wash the precipitate with water several times to neutrality (if it cannot be washed to neutrality, a small amount of NaOH solution can be used to neutralize the acidity). The filtrate was discarded or kept for the next reaction.

[0057] 3.2 Reaction of hydrochloric acid reaction product with cellulase

[0058] Add the above hydrochloric acid reaction product to 250mLNaH 2 PO 4 -Na 2 HPO 4 (pH5.5, 50uM) buffer solution, then add about 5mL of cellulase (comprehensive enzyme activity ≥ 18,000u / mL), and stir at 40°C for 32 hours. After the reaction, cool down, add ...

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Abstract

The invention relates to a preparation method of hydrated icariin which belongs to the synthesis field of natural compounds. The preparation method of the hydrated icariin is characterized in that the hydrated icariin is obtained from icariin after two steps of the hydrolysis reaction of hydrochloride and cellulose. The desugarization hydrolysis is complete. The chemical structure of barrenwort aglycone can be changed, which changes the barrenwort aglycone into the hydrated icariin. The yield is high. The treatment after the reaction is convenient. And the purity of products fully complies with the medical standards.

Description

technical field [0001] The invention relates to the synthesis of natural compounds, in particular to a preparation method of hydrated epimeditin, a component of 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). Namely Epimedium brevicomum Maxim), Epimedium sagittatum, Epimedium pubescens, Epimedium wushanenes, Epimedium koreanum Nakai, etc. . Epimedium has the functions of tonifying 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 activity. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C12P17/06
Inventor 李靖孟坤
Owner BEIJING SHENOGEN BIOMEDICAL
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