CN112062794A - Epimedium extract and preparation process thereof - Google Patents
Epimedium extract and preparation process thereof Download PDFInfo
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- CN112062794A CN112062794A CN202011137960.4A CN202011137960A CN112062794A CN 112062794 A CN112062794 A CN 112062794A CN 202011137960 A CN202011137960 A CN 202011137960A CN 112062794 A CN112062794 A CN 112062794A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
- C07H17/07—Benzo[b]pyran-4-ones
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Abstract
The invention relates to the technical field of epimedium extracts and discloses an epimedium extract and a preparation process thereof, wherein the preparation process comprises the following steps: the preparation method comprises the steps of crushing dried epimedium leaves by using a superfine crusher, adding the crushed epimedium into warm water, heating and concentrating, adding diluted ethanol aqueous solution into concentrated solution, taking the ethanol aqueous solution as an extraction solvent, preserving at constant temperature, continuing heating and concentrating the solution, filtering the concentrated solution by using a microfiltration membrane, and removing impurities in the concentrated solution.
Description
Technical Field
The invention relates to the technical field of epimedium extracts, in particular to an epimedium extract and a preparation process thereof.
Background
With the continuous development of all aspects of society, the living standard of people is continuously improved, but the functions of the immune system of people are weakened, the possibility of attack of various diseases is increased, the possibility of contacting harmful bacteria and viruses is increased, respiratory tract and intestinal tract infection is easy to occur to people, and the incidence rate of rheumatism and bone diseases is increased, so that corresponding medicines are needed to strengthen the immune system of people and improve the body resistance of people.
The epimedium herb is a traditional Chinese medicine for impotence and spermatorrhea, flaccidity of bones and muscles, rheumatic arthralgia and numbness and contracture caused by kidney-yang deficiency, has the efficacies of invigorating kidney yang, strengthening bones and muscles and dispelling wind-damp, and icariin is one of main active ingredients of the epimedium herb, can be used for enhancing the immune system of a human body and improving the physical conditions of people.
In order to solve the problems, the epimedium extract and the preparation process have the advantages of good icariin preparation effect, high preparation yield, high preparation process efficiency and capability of realizing industrial production.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides the epimedium extract and the preparation process thereof, which have the advantages of good icariin preparation effect, high preparation yield, high preparation process efficiency and capability of realizing industrial production, and solve the problems of poor preparation effect, low yield and low preparation efficiency of the existing icariin.
(II) technical scheme
In order to realize the purposes of good preparation effect, high preparation yield, high preparation process efficiency and realization of industrial production of the icariin, the invention provides the following technical scheme: a herba Epimedii extract and its preparation method comprise the following steps:
s1, pulverizing the dried epimedium leaves by using a superfine pulverizer, adding the pulverized epimedium into warm water, and heating and concentrating;
s2, adding the diluted ethanol water solution into the concentrated solution in the S1, taking the ethanol water solution as an extraction solvent, preserving at constant temperature, and then continuing to heat and concentrate the solution;
s3, filtering the concentrated solution in the step S2 by using a micro-filtration membrane to remove impurities in the concentrated solution;
s4, taking macroporous adsorption resin as a solid phase of the filtrate in the S3, firstly carrying out flow elution by using water, then carrying out secondary elution by using an ethanol water solution, and collecting the liquid eluted by the ethanol water solution;
s5, evaporating and drying the eluent collected in the S4 by using a heating pipe to obtain solid particles;
s6, collecting the solid particles in the S5 to obtain the icariin.
Preferably, the heating temperature is kept between 55 ℃ and 70 ℃, the heating time is 25-35min, and the concentration times are 3-5 times.
Preferably, the volume fraction of the ethanol extraction solvent is 60-70%, and the mass ratio of the epimedium leaf to the added ethanol solvent is 1: 8-11, keeping at constant temperature for 5-8h, keeping at 35-45 deg.C, heating at 55-70 deg.C for 25-35min, and concentrating for 3-5 times.
Preferably, the micro-filtration membrane is a micro-filtration membrane with a filtration pore size of 0.35-0.40 μm.
Preferably, the speed of the water flow elution is 0.8-1.2BV/h, and the volume fraction of the ethanol elution aqueous solution is 45% -65%.
Preferably, the heating tube temperature is maintained at 50 to 70 ℃ during the early preheating stage, and then is continuously increased and maintained at 110 to 130 ℃.
(III) advantageous effects
Compared with the prior art, the invention provides the epimedium extract and the preparation process thereof, and the epimedium extract has the following beneficial effects:
1. the herba Epimedii extract is prepared by micronizing and pulverizing folium Epimedii, so as to release effective components in folium Epimedii with high efficiency, and improve extraction yield of icariin.
2. The herba Epimedii extract is prepared by extracting solvent with ethanol, concentrating for several times, and can fully release effective components in herba Epimedii leaf and effectively increase icariin extraction amount.
3. The herba Epimedii extract can remove impurities in the concentrated solution by using microfiltration membrane, and is beneficial for improving purity of icariin.
4. The herba Epimedii extract is prepared by eluting filtrate with water solution and ethanol water solution, and heating in heating tube for stage to ensure purity of icariin.
5. The icariin preparation process is simple, convenient to operate and low in requirements on working conditions, and can realize industrial production.
Drawings
FIG. 1 is a schematic view of the process for preparing icariin of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the following specific embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Weighing 5kg of dried epimedium leaves, and crushing the epimedium leaves into about 50 meshes by using a superfine crusher;
adding warm water, heating at 65 deg.C for 30min, and concentrating for 3 times;
then adding an extraction solvent, wherein the volume fraction of the ethanol aqueous solution extraction solvent is 60%, and the mass ratio of the epimedium leaves to the added ethanol solvent is 1: 8, then preserving at constant temperature for 6 hours at about 40 ℃, keeping the heating temperature at about 65 ℃, heating for 30min, and concentrating for 3 times;
then filtering by using a micro-filtration membrane with the aperture of 0.40 mu m, and taking macroporous adsorption resin as a solid phase;
then, sequentially eluting by using an aqueous solution and an ethanol solution, wherein the flow rate of the aqueous solution is 1VB/h, and the volume fraction of the ethanol aqueous solution is 50%;
then evaporating and crystallizing the elution solution by using a heating pipe, keeping the temperature of the heating pipe at about 60 ℃ in the early preheating stage, and then continuously heating and keeping the temperature at about 120 ℃;
finally, the crystallized particles were collected, and the icariin was weighed as 0.0487kg, and the purity of icariin was 97.3%.
Example 2
Weighing 5kg of dried folium Epimedii, pulverizing folium Epimedii into about 50 mesh with micronizer, adding warm water, heating at about 65 deg.C for 30min, and concentrating for 4 times;
then adding an extraction solvent, wherein the volume fraction of the ethanol aqueous solution extraction solvent is 65%, and the mass ratio of the epimedium leaves to the added ethanol solvent is 1: 9, then preserving at constant temperature for 6 hours at about 40 ℃, keeping the heating temperature at about 65 ℃, heating for 30min, and concentrating for 4 times;
then filtering by using a micro-filtration membrane with the aperture of 0.40 mu m, and taking macroporous adsorption resin as a solid phase;
then, sequentially eluting by using an aqueous solution and an ethanol solution, wherein the flow rate of the aqueous solution is 1.1VB/h, and the volume fraction of the ethanol aqueous solution is 60%;
then evaporating and crystallizing the elution solution by using a heating pipe, keeping the temperature of the heating pipe at about 60 ℃ in the early preheating stage, and then continuously heating and keeping the temperature at about 120 ℃;
finally, the crystallized particles were collected, and the icariin was weighed as 0.0493kg, and the purity of icariin was 97.8%.
Example 3
Weighing 5kg of dried epimedium leaves, and crushing the epimedium leaves into about 50 meshes by using a superfine crusher;
adding warm water, heating at 65 deg.C for 30min, and concentrating for 5 times;
then adding an extraction solvent, wherein the volume fraction of the ethanol aqueous solution extraction solvent is 65%, and the mass ratio of the epimedium leaves to the added ethanol solvent is 1: 10, then preserving at constant temperature for 6 hours at about 40 ℃, keeping the heating temperature at about 65 ℃, heating for 30min, and concentrating for 5 times;
then filtering by using a micro-filtration membrane with the aperture of 0.40 mu m, and taking macroporous adsorption resin as a solid phase;
then, sequentially eluting by using an aqueous solution and an ethanol solution, wherein the flow rate of the aqueous solution is 1.2VB/h, and the volume fraction of the ethanol aqueous solution is 65%;
then evaporating and crystallizing the elution solution by using a heating pipe, keeping the temperature of the heating pipe at about 60 ℃ in the early preheating stage, and then continuously heating and keeping the temperature at about 120 ℃;
finally, the crystallized particles were collected, and icariin was weighed to be 0.0496kg, and the purity of icariin was 98.1%.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. The epimedium extract and the preparation process are characterized by comprising the following steps:
s1, pulverizing the dried epimedium leaves by using a superfine pulverizer, adding the pulverized epimedium into warm water, and heating and concentrating;
s2, adding the diluted ethanol water solution into the concentrated solution in the S1, taking the ethanol water solution as an extraction solvent, preserving at constant temperature, and then continuing to heat and concentrate the solution;
s3, filtering the concentrated solution in the step S2 by using a micro-filtration membrane to remove impurities in the concentrated solution;
s4, taking macroporous adsorption resin as a solid phase of the filtrate in the S3, firstly carrying out flow elution by using water, then carrying out secondary elution by using an ethanol water solution, and collecting the liquid eluted by the ethanol water solution;
s5, evaporating and drying the eluent collected in the S4 by using a heating pipe to obtain solid particles;
s6, collecting the solid particles in the S5 to obtain the icariin.
2. The epimedium extract and the preparation process thereof according to claim 1 are characterized in that: the heating temperature is kept between 55 ℃ and 70 ℃, the heating time is 25-35min, and the concentration times are 3-5 times.
3. The epimedium extract and the preparation process thereof according to claim 1 are characterized in that: the volume fraction of the ethanol extraction solvent is 60-70%, and the mass ratio of the epimedium leaves to the added ethanol solvent is 1: 8-11, keeping at constant temperature for 5-8h, keeping at 35-45 deg.C, heating at 55-70 deg.C for 25-35min, and concentrating for 3-5 times.
4. The epimedium extract and the preparation process thereof according to claim 1 are characterized in that: the micro-filtration membrane is a micro-filtration membrane with the filtration pore size of 0.35-0.40 μm.
5. The epimedium extract and the preparation process thereof according to claim 1 are characterized in that: the speed of water flow elution is 0.8-1.2BV/h, and the volume fraction of the ethanol elution aqueous solution is 45% -65%.
6. The epimedium extract and the preparation process thereof according to claim 1 are characterized in that: the heating tube temperature is kept at 50 ℃ to 70 ℃ in the early preheating stage, and then is continuously increased in temperature and kept at 110 ℃ to 130 ℃.
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| CN202011137960.4A CN112062794A (en) | 2020-10-22 | 2020-10-22 | Epimedium extract and preparation process thereof |
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| CN202011137960.4A CN112062794A (en) | 2020-10-22 | 2020-10-22 | Epimedium extract and preparation process thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113318140A (en) * | 2021-06-11 | 2021-08-31 | 劲牌持正堂药业有限公司 | Low-ash epimedium extract and its grading preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113318140A (en) * | 2021-06-11 | 2021-08-31 | 劲牌持正堂药业有限公司 | Low-ash epimedium extract and its grading preparation method |
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