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Preparation method of epimedium aglycone

A technology of icariin and epimedium, applied in the field of preparation of icariin, can solve problems such as inability to obtain pure icariin, inability to remove glycosidic bonds, complex glycosidic bond structure, etc., to achieve The effect of strong purpose, high conversion rate and simplified operation steps

Inactive Publication Date: 2010-06-30
JIANGSU PROVINCE INST OF TRADITIONAL CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

(2) Biotransformation method, such as using Epimedium as the fermented enzyme inducer of bacteria, molds, and yeasts to prepare a mold-containing liquid, and then use this bacterial liquid to convert Epimedium flavonoid glycosides into low glycosides or glycosides Yuan (publication number: CN1473938A enzymatically hydrolyzing icariin glycosyl to prepare low-sugar icariin or aglycone), because there are many kinds of epimedium flavonoid glycosides, and its glycosidic bond structure is very complicated, mainly composed of α- L-rhamnosidic bonds, β-D-glucosidic bonds, β-D-xyloglycosidic bonds and other monosaccharide glycosidic bonds and disaccharide glycosidic bonds composed of them, plus the high specificity of enzyme-catalyzed hydrolysis , these enzyme-containing bacterial solutions cannot completely remove the glycosidic bonds, so it is impossible to obtain icariin with higher purity
There is no report on the preparation of icariin by using helicase

Method used

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  • Preparation method of epimedium aglycone
  • Preparation method of epimedium aglycone
  • Preparation method of epimedium aglycone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Grind 100 g of dried Epimedium medicinal material, add solvent for reflux extraction twice, add 10 times the amount of 70% ethanol for reflux extraction for 2 hours for the first time, add 8 times the amount of 70% ethanol for reflux extraction for 2 hours for the second time, Concentrate under reduced pressure to obtain 20.3 g of paste; add 1000 mL of acetic acid-sodium acetate buffer solution (pH5.7) to the paste, add 2 g of helicase, put it in a constant temperature oscillating air bath, and heat it at 37 ° C, 100 r / h min reaction for 48 hours. Take the precipitate by centrifugation, wash three times with pure water, 100mL each time, dissolve it with absolute ethanol, filter the filtrate, and wave off the absolute ethanol to obtain 1.12g crude icariin, which is then recrystallized with absolute ethanol to obtain Icariin with a purity greater than 90%. Appearance: yellow powder, ESI-MS positive spectrum gives m / z369[M+H] + , melting point: 232-233°C, 1 H NMR (DMSO,...

Embodiment 2

[0040] Cut 100g of dried epimedium into sections, add solvent for reflux extraction twice, add 8 times the amount of 95% ethanol for reflux extraction for 2 hours for the first time, add 6 times the amount of 95% ethanol for reflux extraction for 2 hours for the second time , concentrated under reduced pressure to obtain 20.1 g of paste; add 201 mL of acetic acid-sodium acetate buffer solution (pH 3.5) to the paste, add 100.5 g of helicase, put it in a constant temperature oscillating air bath, and heat it at 15 ° C. 100r / min reaction for 72 hours. The precipitate was collected by centrifugation and washed with pure water three times, 100 mL each time, dissolved in absolute ethanol, filtered to obtain the filtrate, and the absolute ethanol was evaporated to obtain 1.10 g of icariin. Use D101 macroporous resin (provided by Nankai University Chemical Factory) column chromatography, elute with 40% ethanol until the eluate is colorless, discard, then elute icariin with 95% ethanol...

Embodiment 3

[0043] Grind 100 g of dried Epimedium medicinal material, add solvent for reflux extraction twice, add 20 times the amount of 30% ethanol for reflux extraction for 2 hours for the first time, add 15 times the amount of 30% ethanol for reflux extraction for 2 hours for the second time, Concentrate under reduced pressure to obtain 18.3 g of paste; add 1830 mL of acetic acid-sodium acetate buffer solution (pH9.0) to the paste, add 91.5 g of helicase, put it in a constant temperature oscillating air bath, and heat it at 15 ° C and 100 r / min for 2 hours. Centrifuge the precipitate and wash it with pure water three times, 100mL each time, dissolve it with absolute ethanol, filter the filtrate, and wave off the absolute ethanol to obtain 1.02g of crude icariin, which is then recrystallized with ethyl acetate and dried 0.91 g of icariin was obtained, which was the same compound as in Example 1. The purity of icariin was detected by HPLC to be higher than 90%, and the melting point wa...

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Abstract

The invention relates to a preparation method of epimedium aglycone, which comprises the steps that dried epimedium is pulverized or cut into segments, 30-95% ethanol or 30-100% methanol is added for reflux extraction, the extract solution is decompressed and concentrated to obtain paste, 10-100 ml of acetate-sodium acetate buffer solution with the pH of 3.5-9.0 is added into each gram of paste, snailase is added for hydrolysis, the mass ratio of enzyme to paste is 0.05-5, the reaction temperature is 15 to 80 DEG C, the reaction time is 2 to 72h, the reaction solution is centrifuged, the precipitate is dissolved with an organic solvent, filtration is carried out to obtain filtrate, the solvent is steamed away to obtain crude epimedium aglycone, and pure epimedium aglycone is obtained after recrystallization. The invention has the characteristic that the epimedium extract is directly converted into high-purity aglycone in one step by utilizing the strong enzymic hydrolysis of the snailase so as to simplify the operation steps with strong purposiveness and high conversion rate, and has the advantages of no pollution and large-scale production. The invention overcomes the shortcomings of large destruction on the aglycone, serious pollution, poor purposiveness, low conversion rate, difficult separation and purification and the like of the prior art.

Description

Technical field: [0001] The invention belongs to the field of natural medicines and relates to a preparation method of icariin. Background technique: [0002] Epimedium was first recorded in "Shen Nong's Materia Medica", which has the functions of nourishing kidney and strengthening yang, dispelling wind and dampness, strengthening muscles and strengthening bones, etc. It is clinically used to treat osteoporosis caused by various reasons. Experiments have shown that the flavonoid components of Epimedium are the effective parts of its anti-osteoporosis, and the active ingredient icarigenin has the most obvious effect, which can promote the activity of osteoblasts and inhibit the activity of osteoclasts in vitro. Therefore, the preparation of Epimedium Amarigenin is of great value in the development of new anti-osteoporosis drugs. [0003] Icaritin, full name 3,5,7-trihydroxy-4′-methoxy-8-prenyl flavone, also known as icaritin, English name Icaritin, is a class of polyhydroxy...

Claims

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Application Information

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IPC IPC(8): C12P17/06
Inventor 贾晓斌贾东升孙娥
Owner JIANGSU PROVINCE INST OF TRADITIONAL CHINESE MEDICINE
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