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Method for enriching and purifying icariin in epimedium herb

A technology of icariin and epimedium, which is applied to the purification of icariin, uses batch distillation-macroporous adsorption resin coupling method to enrich and purify icariin in epimedium, and can solve the problem of low extraction purity. , low extraction rate and other problems, to achieve the effect of high extraction purity, large adsorption capacity and obvious separation effect

Inactive Publication Date: 2011-05-25
DAXINGANLING LINGOBERRY BOREAL BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the shortcomings of conventional techniques such as relatively low extraction rate and low extraction purity, and provide a method for enriching and purifying icariin in epimedium by using batch distillation-macroporous adsorption resin coupling method

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0025] Embodiment 1: a kind of method that utilizes batch distillation-macroporous adsorption resin coupling method to enrich and purify icariin in Epimedium herba, its steps are as follows:

[0026] (1) crush the dried Epimedium and pass through a 60-mesh sieve, then reflux and extract the dried Epimedium according to the ratio of material: 75% ethanol = 1:6, 4 hours each time;

[0027] (2) The extracts are mixed, suction filtered, and concentrated under reduced pressure to recover ethanol to obtain the initial extract;

[0028] (3) Extract the obtained primary extract with purified water, adjust the pH to 2.0, let stand, and filter with suction to obtain the crude icariin extract;

[0029] (4) The obtained icariin extract is adsorbed on a macroporous adsorption resin chromatography column, and the macroporous resin used is NKA-II type resin produced by Tianjin Nankai University;

[0030] (5) Use 30%, 40%, 50%, 60%, 70%, 80%, 90% ethanol to carry out gradient elution in sequ...

Embodiment example 2

[0034] Implementation Case 2: A method for enriching and purifying icariin in Epimedium using batch distillation-macroporous adsorption resin coupling method, the steps are as follows:

[0035] (1) crush the dried Epimedium and pass through a 80-mesh sieve, and extract the dried Epimedium according to the material: 85% ethanol = 1:6 reflux twice, each time for 4 hours;

[0036] (2) The extracts are mixed, suction filtered, and concentrated under reduced pressure to recover ethanol to obtain the initial extract;

[0037] (3) Extract the obtained primary extract with purified water, adjust the pH to 2.3, let stand, and suction filter to obtain the crude icariin extract;

[0038] (4) The obtained icariin crude extract is adsorbed with a macroporous adsorption resin, and the macroporous resin used is the D4006 type resin produced by Tianjin Nankai University;

[0039] (5) Elute with 30%, 50%, 70%, 90% ethanol on the macroporous adsorption resin, track and detect with thin-layer c...

Embodiment example 3

[0043] Implementation Case 3: A method for enriching and purifying icariin in Epimedium Herba using batch distillation-macroporous adsorption resin coupling method, the steps are as follows:

[0044] (1) crush the dried Epimedium and pass through a 40-mesh sieve, then reflux and extract the dried Epimedium according to the ratio of material: 80% ethanol = 1:6, 4 hours each time;

[0045] (2) The extracts are mixed, suction filtered, and concentrated under reduced pressure to recover ethanol to obtain the initial extract;

[0046] (3) Extract the obtained primary extract with purified water, adjust the pH to 2.5, let stand, and suction filter to obtain the crude icariin extract;

[0047] (4) The obtained icariin crude extract is adsorbed on a macroporous adsorption resin chromatography column, and the macroporous resin used is the NKA-9 type resin produced by Tianjin Nankai University;

[0048] (5) Use 40%, 60%, and 80% ethanol to sequentially perform gradient elution in the m...

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Abstract

The invention belongs to the field of natural organic chemistry and relates to a method for enriching and purifying icariin in epimedium herb by a batch distillation-macro absorption resin coupling method. The method is characterized in that: icariin is separated and purified by the batch distillation-macro absorption resin coupling method, the adsorption selectivity to icariin is high, adsorption and resolution are quick and adsorption volume is large; and extraction is convenient and quick, raw materials are readily available, production cost is low, separation effect is remarkable, extraction purity is high, an icariin semi-finished product with the icariin content of over 35 percent and an icariin finished product with the icariin content of over 95 percent can be obtained, and the defects of low extraction rate and low extraction purity by the conventional method are overcome. Macro absorption resin with stable physicochemical property, a large surface area, high exchange speed, high mechanical strength, high contamination resistance and high thermal stability is used, so that icariin is selectively adsorbed from solution by physical adsorption, adsorption and resolution are quick, and adsorption volume is large.

Description

Technical field: [0001] The invention belongs to the field of natural organic chemistry and relates to a method for purifying icariin, in particular to a method for enriching and purifying icariin in epimedium by a batch distillation-macroporous adsorption resin coupling method. Background technique: [0002] Epimedium: also known as fairy spleen, three-branch nine-leaf grass, lung meridian grass, ox horn flower, etc., it is the dry aerial part of Epimedium cordifolia, Epimedium pubescens, and Epimedium vellus. Epimedium leaves and stems contain icariin (Icariin), icariside (Icariside), des-O-Methylicariin (des-O-Methylicariin), β-dehydroicariin (β-anhy-Droicaritin), Epimedoside (Epimedoside) A, B, C, D, E. have androgen-like effects, anti-aging effects, and can play a certain role in the immune system and cardiovascular system . [0003] Icariin is the dry stem and leaf extracts of Epimedium sagitta, Epimedium pilosa, and Epimedium wushanense. It has been proved by scient...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/08
Inventor 姚德坤姚德利闫峰黄运生姚航郑君
Owner DAXINGANLING LINGOBERRY BOREAL BIOTECH CO LTD
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