CN113943335A - Preparation process of herba Cymbopogonis Citrari extract - Google Patents

Preparation process of herba Cymbopogonis Citrari extract Download PDF

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CN113943335A
CN113943335A CN202111409171.6A CN202111409171A CN113943335A CN 113943335 A CN113943335 A CN 113943335A CN 202111409171 A CN202111409171 A CN 202111409171A CN 113943335 A CN113943335 A CN 113943335A
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extract
eluent
ecdysterone
beta
adsorption column
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何文祥
李俊华
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Yunnan Xicao Biotechnology Development Co ltd
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    • C07ORGANIC CHEMISTRY
    • C07JSTEROIDS
    • C07J9/00Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of more than two carbon atoms, e.g. cholane, cholestane, coprostane

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract

A preparation process of a herba Cymbopogonis Citrari extract belongs to the technical field of plant component extraction. The preparation process comprises the following steps: mixing herba Eragrostidis and extractant, and extracting under hot reflux to obtain extractive solution; putting the extracting solution into a first adsorption column with macroporous resin, so that the macroporous resin adsorbs the beta-ecdysterone; eluting the macroporous resin in the first adsorption column by using an eluent, and collecting a first eluent containing beta-ecdysterone; and (3) putting the first eluent into a second adsorption column with ion exchange resin for impurity removal, and collecting a second eluent containing the beta-ecdysterone. The method can effectively remove impurities and improve the content and yield of the beta-ecdysterone.

Description

Preparation process of herba Cymbopogonis Citrari extract
Technical Field
The application relates to the technical field of plant component extraction, in particular to a preparation process of a herba Cymbopogonis Citrari extract.
Background
Herba Cymbopogonis Citrari is a perennial herb of the genus Cyperus of the family Plantaginaceae, also known as Codonopsis lanceolata, Euphorbia pulcherrima, Largeflower Millettia, Ruyi and Ecliptae herba, with root fibrous shape. The beta-ecdysterone rich in the Cyanotis pseudolaris has extremely high application value and is widely applied to the industries of cultivation, health care, cosmetics and medicines.
The existing extraction and separation process of beta-ecdysterone mainly adopts a solvent extraction method, and the method is simple and convenient to operate, but has low product yield and serious environmental pollution. For example, some existing methods for extracting and purifying the beta-ecdysterone-rich dew grass adopt primary resin adsorption and recrystallization, and the specific processes are that the dew grass is sequentially subjected to water reflux extraction, alcohol precipitation, macroporous resin adsorption, extraction by ethyl acetate and concentration crystallization, silica gel column chromatography and purification. The method needs alcohol precipitation, and ethyl acetate is adopted for recrystallization. However, in the research of the inventors of the present application, it was found that, since the rhizomes of the plant aquatilis contain various aglycones, glycosides, sterones, sugars, etc., the extract obtained by extracting with water and then separating and purifying with macroporous resin is very viscous, since the extract is difficult to disperse and wraps with water to form a heterogeneous solution, when beta-ecdysterone is extracted with ethyl acetate in the process, an emulsion is easily formed, the extraction efficiency is reduced, and other impurities are easily introduced. On the other hand, ethyl acetate is difficult to permeate into suspension (heterogeneous solution), cannot effectively extract and enrich beta-ecdysterone wrapped in the suspension, and is often extracted for more than 6-7 times in actual production. Even so, a large part of beta-ecdysterone still cannot be extracted and enriched, and the product yield is low. In addition, the ethyl acetate used in the production process is a polar solvent, is volatile and toxic, and is easy to cause harm to the environment and operators.
Disclosure of Invention
The application provides a preparation process of a herba Cymbopogonis Citrari extract, which can effectively remove impurities, improve the content and yield of beta-ecdysterone, and can solve the problems that the use of ethyl acetate in the prior art causes harm to the environment and influences the health of operators.
The embodiment of the application is realized as follows:
the embodiment of the application provides a preparation process of a dew grass extract, which comprises the following steps:
mixing herba Eragrostidis and extractant, and extracting under hot reflux to obtain extractive solution;
putting the extracting solution into a first adsorption column with macroporous resin, so that the macroporous resin adsorbs the beta-ecdysterone; eluting the macroporous resin in the first adsorption column by using an eluent, and collecting a first eluent containing beta-ecdysterone;
and (3) putting the first eluent into a second adsorption column with ion exchange resin for impurity removal, and collecting a second eluent containing the beta-ecdysterone.
The preparation process of the dew grass extract provided by the embodiment of the application has the beneficial effects that:
the beta-ecdysterone in the herba Cymbopogonis Citrari can be effectively extracted by mixing the extractant with the herba Cymbopogonis Citrari and then carrying out hot reflux extraction, but other impurities can also be mixed in the extraction process. Placing the extract in a first adsorption column with macroporous resin, wherein the macroporous resin can adsorb beta-ecdysterone in the extract and can remove a part of impurities such as polysaccharide, protein, amino acid and the like, but can not remove other impurities such as pigment and the like. The macroporous resin in the first adsorption column is eluted by an eluent to obtain a first eluent containing beta-ecdysterone, the first eluent also contains impurities which are not removed by the first adsorption column, the first eluent is placed in a second adsorption column with ion exchange resin, the first eluent absorbs the impurities by the ion exchange resin, the impurities such as pigment are removed to obtain a second eluent, the impurities are effectively removed, and the content and the yield of the beta-ecdysterone are obviously improved. In addition, the beta-ecdysterone is not required to be extracted by ethyl acetate, and the problems that the environmental pollution is caused and the health of operators is influenced by the use of ethyl acetate in the prior art can be solved.
Detailed Description
Embodiments of the present application will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present application and should not be construed as limiting the scope of the present application. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following is a detailed description of the preparation process of the extract of the dewy grass in the examples of the present application:
the embodiment of the application provides a preparation process of a dew grass extract, which comprises the following steps:
(1) mixing herba Eragrostidis and extractant, and extracting under hot reflux to obtain extractive solution.
The beta-ecdysterone in the herba Cymbopogonis Citrari can be effectively extracted by mixing the extractant with the herba Cymbopogonis Citrari and then carrying out hot reflux extraction. Optionally, the embodiment of the present application selects rhizomes of the dewy grass, wherein leaves of the dewy grass may also be selected.
Illustratively, the extract is prepared by pulverizing herba Cymbopogonis Citrari into coarse powder before mixing with the extract to facilitate extraction of effective components.
Illustratively, the weight of the extractant is 3-6 times, e.g., 3 times, 4 times, 5 times, or 6 times the weight of the dew grass.
In some embodiments, the temperature of the hot reflux extraction is 60-100 ℃, and the beta-ecdysterone can be extracted more favorably under the temperature condition. Optionally, the temperature of the hot reflux extraction is 60 ℃, 70 ℃, 80 ℃, 90 ℃ or 100 ℃.
Illustratively, the extraction times of the hot reflux are 2-4 times, each time is 0.5-3 h, and after multiple extractions, the extraction liquids obtained by the multiple extractions are combined.
In some embodiments, the extractant includes at least one of an alcohol, a ketone, and water. That is, the extractant may be alcohol, ketone or water alone, or an aqueous alcohol solution, an aqueous ketone solution or an aqueous solution containing both of ketone and alcohol.
Optionally, the alcohol comprises at least one of ethanol and methanol. Optionally, the ketone species comprises acetone.
When the extractant contains alcohol substances and/or ketone substances, the extracting solution is concentrated and evaporated to obtain extract, and then the subsequent operation is carried out. After the extracting solution is concentrated and evaporated, alcohol substances and/or ketone substances can be evaporated, so that the influence of the alcohol substances and/or ketone substances on subsequent processes is reduced, and the yield is improved. In addition, the temperature of the extractive solution or extract is kept below 40 deg.C.
(2) Putting the extracting solution into a first adsorption column with macroporous resin, so that the macroporous resin adsorbs the beta-ecdysterone; eluting the macroporous resin in the first adsorption column by using an eluent, and collecting a first eluent containing the beta-ecdysterone.
During the process of extracting the dewed grass by using the extracting agent, the obtained extracting solution is mixed with other impurities.
Placing the extract in a first adsorption column with macroporous resin, wherein the macroporous resin can adsorb beta-ecdysterone in the extract and can remove a part of impurities such as polysaccharide, protein, amino acid and the like, but can not remove other impurities such as pigment and the like. And eluting the macroporous resin in the first adsorption column by using an eluent to obtain a first eluent containing the beta-ecdysterone, wherein the first eluent also contains impurities which are not removed by the first adsorption column.
Optionally, when the extractant used in step (1) contains alcohols and/or ketones, the extract is concentrated and evaporated to obtain an extract, and then the extract is placed in the first adsorption column with macroporous resin.
When the extractant contains alcohol substances and/or ketone substances, the obtained extracting solution also contains the alcohol substances and/or ketone substances, and then if the extracting solution is placed in a first adsorption column with macroporous resin for adsorption, the adsorption of the macroporous resin on the beta-ecdysterone is influenced, so that the product yield is influenced.
In some embodiments, the eluent comprises at least one of an alcohol, a ketone, and water. That is, the eluent may be selected from an alcohol, a ketone, or water alone, an alcohol aqueous solution, a ketone aqueous solution, or a mixture of a ketone and an alcohol aqueous solution. The beta-ecdysterone adsorbed by the macroporous resin can be effectively eluted by utilizing the eluent.
Optionally, the alcohol comprises at least one of ethanol and methanol. Optionally, the ketone species comprises acetone.
Illustratively, in some possible embodiments, the eluent comprises a ketone substance and an alcohol substance in a mass ratio of 1-9: 1-9. For example, the mass ratio of the ketone substance to the alcohol substance is 1: 9. 2:8, 3:7, 4:6, 5:5, 6:4, 7:3, 8:2, or 9: 1.
Optionally, the eluent is an aqueous alcohol solution, and the mass percentage concentration of the alcohol in the aqueous alcohol solution is 10-90%, for example, 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80% or 90%.
Optionally, the mass of the eluent is 2-5 times of the mass of the extract or the extracting solution.
(3) And (3) putting the first eluent into a second adsorption column with ion exchange resin for impurity removal, and collecting a second eluent containing the beta-ecdysterone.
The first eluent contains impurities which are not removed by the first adsorption column, the first eluent is placed in a second adsorption column with ion exchange resin, the first eluent passes through the ion exchange resin to adsorb the impurities, and the impurities such as pigment and the like are removed to obtain a second eluent, the impurities are effectively removed, and the yield of the beta-ecdysterone is obviously improved. In addition, the beta-ecdysterone is not required to be extracted by ethyl acetate, so that the problem of harm to the environment and operators can be solved.
The ion exchange resin may be cation exchange resin or anion exchange resin. The research of the inventor of the application finds that the anion exchange resin adopted in the second adsorption column has better impurity removal effect than the cation exchange resin, and is more favorable for improving the product yield and content of the beta-ecdysterone. Wherein the anion exchange resin can be at least one of styrene anion exchange resin and acrylic anion exchange resin. For example, there may be mentioned macroporous strongly basic styrene type anion exchange resins (e.g., D201), macroporous II strongly basic styrene type anion exchange resins (e.g., D202), macroporous weakly basic styrene type anion exchange resins (e.g., D301), and macroporous acrylic weakly acidic anion exchange resins (e.g., D318); at least one of macroporous styrene series weak base anion exchange resin (such as D314) and macroporous acrylic series weak base anion exchange resin (such as D311, D941).
Wherein the cation exchange resin can be selected from quaternary ammonium type cation exchange resin, styrene type anion exchange resin and acrylic cation exchange resin, such as at least one of macroporous strong basic quaternary ammonium type cation exchange resin (such as D254), macroporous strong acid styrene type cation exchange resin (such as D-62) and macroporous acrylic weak acid cation exchange resin (such as D-85).
(4) And concentrating the second eluent containing the beta-ecdysterone to obtain thick paste, and drying the thick paste.
When the first eluent contains alcohol or ketone, the second eluent is concentrated to remove alcohol, ketone and water, and the thick paste is dried to obtain a finished product with high content of beta-ecdysterone. For example, the thick paste may be dried and then subjected to a pulverization treatment. Tests show that the content of beta-ecdysterone in the dried product is more than 53 percent.
The preparation process of the extract of the dewy grass of the present application is further described in detail with reference to the following examples.
Example 1
The present embodiment provides a preparation process of a herbal extract, which includes the following steps:
pulverizing the rhizome of herba Eragrostidis Pendulae into granules, adding 10kg of ethanol aqueous solution with weight percentage concentration of 50% 5 times of the weight of the rhizome of herba Eragrostidis Pendulae as extractant, and extracting under reflux at 80 deg.C for 3 times, each for 2 hr; mixing the extractive solutions, filtering the mixed extractive solutions, recovering alcohol solution, concentrating the alcohol solution, and evaporating until there is no alcohol to obtain extract. Keeping the temperature of the extract below 40 ℃ for later use.
Pouring the extract into a first adsorption column filled with polar macroporous adsorption resin, eluting the first adsorption column by using 80 wt% of ethanol aqueous solution as an eluent, wherein the mass of the eluent is 4 times that of the extract, and collecting a first eluent containing beta-ecdysterone after elution.
Pouring the first eluent into a second adsorption column filled with macroporous acrylic weakly-basic anion exchange resin (D311) for adsorption and impurity removal, and collecting a second eluent containing beta-ecdysterone.
Concentrating the second eluate to obtain soft extract, drying the soft extract, and pulverizing to obtain herba Eragrostidis Pendulae extract containing beta-ecdysterone.
Example 2
The present embodiment provides a preparation process of a herbal extract, which includes the following steps:
pulverizing the rhizome of herba Eragrostidis Pendulae into granules, adding 10kg of ethanol aqueous solution with weight percentage concentration of 80% 5 times of the weight of the rhizome of herba Eragrostidis Pendulae as extractant, and extracting under reflux at 70 deg.C for 3 times, each for 2 hr; mixing the extractive solutions, filtering the mixed extractive solutions, recovering alcohol solution, concentrating the alcohol solution, and evaporating until there is no alcohol to obtain extract. Keeping the temperature of the extract below 40 ℃ for later use.
Pouring the extract into a first adsorption column filled with nonpolar macroporous adsorption resin, eluting the first adsorption column by using 80 wt% ethanol aqueous solution as an eluent, wherein the mass of the eluent is 4 times that of the extract, and collecting a first eluent containing beta-ecdysterone after elution.
Pouring the first eluent into a second adsorption column filled with macroporous acrylic weakly-basic anion exchange resin (D311) for adsorption and impurity removal, and collecting a second eluent containing beta-ecdysterone.
Concentrating the second eluate to obtain soft extract, drying the soft extract, and pulverizing to obtain herba Eragrostidis Pendulae extract containing beta-ecdysterone.
Example 3
The present embodiment provides a preparation process of a herbal extract, which includes the following steps:
pulverizing the rhizome of herba Eragrostidis Pendulae into granule, adding 10kg of water 5 times of the weight of the rhizome of herba Eragrostidis Pendulae, and extracting at 100 deg.C under reflux for 2 hr for 3 times; mixing the extractive solutions, filtering the mixed extractive solutions, recovering ethanol, concentrating the ethanol, and evaporating to obtain extract. Keeping the temperature of the extract below 40 ℃ for later use.
Pouring the extract into a first adsorption column filled with nonpolar macroporous adsorption resin, eluting the first adsorption column by using 80 wt% ethanol aqueous solution as an eluent, wherein the mass of the eluent is 4 times that of the extract, and collecting a first eluent containing beta-ecdysterone after elution.
Pouring the first eluate into a second adsorption column filled with macroporous acrylic acid series weakly acidic anion exchange resin (such as D318) for adsorption impurity removal, and collecting second eluate containing beta-ecdysterone.
Concentrating the second eluate to obtain soft extract, drying the soft extract, and pulverizing to obtain herba Eragrostidis Pendulae extract containing beta-ecdysterone.
Example 4
This example provides a process for preparing a herba luodii extract, which is different from example 1 only in that the eluent in this example is a mixture of methanol, acetone and water in a weight ratio of 20:60: 20.
Example 5
This example provides a process for preparing a herba luodii extract, which is different from example 1 only in that the eluent in this example is a mixture of methanol, acetone and water in a weight ratio of 70:10: 20.
Example 6
This example provides a process for preparing a herba luodii extract, which is different from example 2 only in that the eluent in this example is a mixture of methanol, acetone and water in a weight ratio of 20:60: 20.
Example 7
This example provides a process for preparing a herba luodii extract, which is different from example 1 only in that the extractant in this example is an aqueous ethanol solution with a mass percentage concentration of 80%.
Example 8
This example provides a process for preparing a extract of Cyanotis dahurica, which is different from that of example 1 only in that the extractant of this example is water.
Example 9
This example provides a process for preparing a herba luodii extract, which is different from that of example 2 only in that the extractant of this example is a 50% ethanol aqueous solution.
Example 10
This example provides a process for preparing a extract of Cyanotis dahurica, which is different from that of example 2 only in that the extractant of this example is water.
Examples 11 to 13
Examples 11 to 13 each provide a process for producing a dew grass extract, which is different from example 1 only in that the ion exchange resins of examples 11 to 13 are different from example 1, wherein the ion exchange resins of examples 11 to 13 are a macroporous strongly basic quaternary ammonium type cation exchange resin (D254), a macroporous strongly acidic styrene type cation exchange resin (D-62), and a macroporous acrylic weakly acidic cation exchange resin (D-85), respectively.
Comparative example 1
The comparative example provides a preparation process of a dew grass extract, which comprises the following steps:
pulverizing the rhizome of herba Eragrostidis Pendulae into granules, adding 10kg of ethanol aqueous solution with weight percentage concentration of 50% 5 times of the weight of the rhizome of herba Eragrostidis Pendulae as extractant, and extracting under reflux at 80 deg.C for 3 times, each for 2 hr; mixing the extractive solutions, filtering the mixed extractive solutions, recovering alcohol solution, concentrating the alcohol solution, and evaporating until there is no alcohol to obtain extract. Keeping the temperature of the extract below 40 ℃ for later use.
Pouring the extract into a first adsorption column filled with polar macroporous adsorption resin, eluting the first adsorption column by using 80 wt% of ethanol aqueous solution as an eluent, wherein the mass of the eluent is 4 times that of the extract, and collecting a first eluent containing beta-ecdysterone after elution.
Concentrating the first eluent to thick paste, drying the thick paste to obtain a crude product, adding ethyl acetate with the mass of 5 times of the crude product into the crude product, dissolving, crystallizing, filtering, drying and crushing to obtain the dew-water plant extract containing the beta-ecdysterone.
Comparative example 2
The comparative example provides a preparation process of a dew grass extract, which comprises the following steps:
pulverizing the rhizome of herba Eragrostidis Pendulae into granules, adding 10kg of ethanol aqueous solution with weight percentage concentration of 80% 5 times of the weight of the rhizome of herba Eragrostidis Pendulae as extractant, and extracting under reflux at 70 deg.C for 3 times, each for 2 hr; mixing the extractive solutions, filtering the mixed extractive solutions, recovering alcohol solution, concentrating the alcohol solution, and evaporating until there is no alcohol to obtain extract. Keeping the temperature of the extract below 40 ℃ for later use.
Pouring the extract into a first adsorption column filled with nonpolar macroporous adsorption resin, eluting the first adsorption column by using 80 wt% ethanol aqueous solution as an eluent, wherein the mass of the eluent is 4 times that of the extract, and collecting a first eluent containing beta-ecdysterone after elution.
Concentrating the first eluent to thick paste, drying the thick paste to obtain a crude product, adding ethyl acetate with the mass of 5 times of the crude product into the crude product, dissolving, crystallizing, filtering, drying and crushing to obtain the dew-water plant extract containing the beta-ecdysterone.
Comparative example 3
The present embodiment provides a preparation process of a herbal extract, which includes the following steps:
pulverizing the rhizome of herba Eragrostidis Pendulae into granule, adding 10kg of water 5 times of the weight of the rhizome of herba Eragrostidis Pendulae, and extracting at 100 deg.C under reflux for 2 hr for 3 times; mixing the extractive solutions, filtering the mixed extractive solutions, recovering ethanol, concentrating the ethanol, and evaporating to obtain extract. Keeping the temperature of the extract below 40 ℃ for later use.
Pouring the extract into a first adsorption column filled with nonpolar macroporous adsorption resin, eluting the first adsorption column by using 80 wt% ethanol aqueous solution as an eluent, wherein the mass of the eluent is 4 times that of the extract, and collecting a first eluent containing beta-ecdysterone after elution.
Concentrating the first eluent to thick paste, drying the thick paste to obtain a crude product, adding ethyl acetate with the mass of 5 times of the crude product into the crude product, dissolving, crystallizing, filtering, drying and crushing to obtain the dew-water plant extract containing the beta-ecdysterone.
Test example 1
The mass W of the extract prepared by the preparation process of the dew grass extract of the embodiments 1 to 13 and the comparative examples 1 to 31The test was performed, and the results are shown in table 1.
Evaporating and concentrating the first eluate obtained in the preparation process of the extract of the dewy grass of examples 1 to 13, drying to obtain a first dry substance, and adjusting the mass W of the first dry substance2The weighing was performed, and the results are shown in table 1. Coarse in comparative examples 1 to 3Mass W of product2The weighing was performed, and the results are shown in table 1.
Mass W of the extract of the dew grass of examples 1 to 13 and comparative examples 1 to 33The test was performed, and the results are shown in table 1. Wherein the yield of the finished product is W3Adding rhizome weight W of herba Cymbopogonis Citrari0The transfer rate of the intermediate product to the final product is W3/W2
The content of beta-ecdysterone contained in the extract of the herba aquaticae of examples 1 to 13 and comparative examples 1 to 3 was determined, and the content of beta-ecdysterone in the extract of the herba aquaticae was determined by a high performance liquid chromatograph (appendix 512) according to the high performance liquid chromatography with reference to the detection method of the extract of the herba aquaticae in the book "pharmacopoeia of the people's republic of china". The test method specifically comprises the following steps:
chromatographic condition and system adaptability test: octadecylsilane chemically bonded silica is used as a filling agent; acetonitrile-methanol-water (1:2:4) is used as a mobile phase; the detection wavelength is 243mm, and the number of theoretical plates is not lower than 2500 calculated according to the peak of beta-ecdysone;
preparation of control solutions: taking a proper amount of beta-ecdysone reference substance, precisely weighing, placing into a measuring flask, and adding methanol to obtain a solution containing 0.3mg of beta-ecdysone in each 1 ml;
preparation of a test solution: taking 30mg of a test sample, precisely weighing, placing in a 50ml measuring flask, adding methanol for dissolving, diluting to scale, shaking up, and filtering to obtain the final product;
precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into high performance liquid chromatograph, and measuring.
Figure BDA0003373576890000121
From the results of comparative examples 1 to 13 and comparative examples 1 to 3, it can be seen that the yield of the product in examples 1 to 13 is higher than that in comparative examples 1 to 3, and the content of the product in examples 1 to 13 is higher than that in comparative examples 1 to 3. The preparation process disclosed by the embodiment of the application is more beneficial to improving the extraction rate of the beta-ecdysterone and the yield of the beta-ecdysterone. Reducing the production cost of the dew grass extract.
From the results of comparative examples 1 to 3 and examples 11 to 13, it can be seen that the yield of the final product in examples 1 to 3 is higher in examples 11 to 13, which indicates that the use of anion exchange resin in the second adsorption column is more advantageous for increasing the purity of beta-ecdysterone and increasing the yield of beta-ecdysterone.
The foregoing is illustrative of the present application and is not to be construed as limiting thereof, as numerous modifications and variations will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims (10)

1. A preparation process of a dew grass extract is characterized by comprising the following steps:
mixing herba Eragrostidis and extractant, and extracting under hot reflux to obtain extractive solution;
putting the extracting solution into a first adsorption column with macroporous resin, so that the macroporous resin adsorbs beta-ecdysterone; eluting the macroporous resin in the first adsorption column by using an eluent, and collecting a first eluent containing beta-ecdysterone;
and (3) putting the first eluent into a second adsorption column with ion exchange resin for impurity removal, and collecting a second eluent containing the beta-ecdysterone.
2. The process of claim 1, wherein the ion exchange resin is an anion exchange resin.
3. The process of claim 2, wherein the anion exchange resin comprises at least one of a styrenic anion exchange resin and an acrylic anion exchange resin.
4. The process for preparing a dew grass extract according to any one of claims 1 to 3, wherein the extractant comprises at least one of alcohols, ketones and water.
5. The preparation process of the dew grass extract as claimed in claim 4, wherein the extractant contains alcohol substances and/or ketone substances, the extracting solution is concentrated and evaporated to obtain an extract, and then the extract is put into the first adsorption column with macroporous resin.
6. The process for preparing the dew grass extract as claimed in any one of claims 1 to 3, wherein the temperature of the hot reflux extraction is 60 to 100 ℃.
7. The process for preparing the extract of the aquatic weed according to any one of claims 1 to 3, wherein the eluent comprises at least one of alcohols, ketones and water.
8. The preparation process of the dew grass extract as claimed in claim 7, wherein the eluent comprises a ketone substance and an alcohol substance in a mass ratio of 1-9: 1-9.
9. The preparation process of the dew grass extract as claimed in claim 7, wherein the eluent is an aqueous alcohol solution, and the mass percentage concentration of the alcohol in the aqueous alcohol solution is 10-90%.
10. The preparation process of the dew grass extract as claimed in any one of claims 1 to 3, further comprising: and concentrating the second eluent containing the beta-ecdysterone to obtain thick paste, and drying the thick paste.
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Application publication date: 20220118