Coptis chinensis extraction process
Through degreasing pretreatment, ultrasonic extraction, chitosan flocculation, non-polar macroporous resin adsorption and membrane separation technologies, the problems of impurity removal difficulty and pigment effects in the existing Coptis chitosan extraction process are solved, and efficient Coptis chitosan extraction and purification are achieved to obtain high-purity Coptis chitosan extract.
Patent Information
- Application Number
- CN202510917169.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-03
- Publication Date
- 2025-08-15
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
In the existing Coptis chinensis extraction process, it is difficult to remove impurities, especially the formation of hydrogen bond complexes between polysaccharides and berberine, which leads to co-precipitation of berberine during the alcohol precipitation process, and pigments and berberine form colloids, reducing the adsorption efficiency of resin.
The degreasing pretreatment, ultrasonic extraction, chitosan flocculation, non-polar macroporous resin adsorption, membrane separation and acid-base precipitation methods are adopted, and the fat-soluble and water-soluble impurities are removed and the alkaloid components are retained.
Effectively remove fat-soluble and water-soluble impurities, improve resin adsorption efficiency, reduce berberine loss, and obtain high-purity Coptis extract.
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Figure CN120478464A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of traditional Chinese medicine extraction, in particular to a process for extracting coptis root. Background Art
[0002] Coptis chinensis is a perennial herbaceous plant of the genus Coptis in the family Ranunculaceae. Its leaves are long-stalked, thinly leathery, ovate-pentagonal, heart-shaped at the base, with all lobes petiolated and the middle lobe rhombus-ovate, deeply pinnate, and with fine thorn tips; its bracts are narrow and pinnate; its sepals are yellow-green, lanceolate, its petals are linear-lanceolate, and its fruit is oblong.
[0003] Coptis chinensis extract is a natural ingredient extracted from the rhizome of Coptis chinensis. The main active ingredient is berberine (berberine), which has multiple functions in cosmetics.
[0004] The current Coptidis Rhizoma extraction process still has the following technical problems when preparing Coptidis Rhizoma extracts:
[0005] The current extraction process is difficult to remove impurities in the extract. Polysaccharides in Coptis chinensis (such as Coptis chinensis polysaccharide) form hydrogen bond complexes with berberine. The polysaccharide content in the aqueous extract can be 2-3 times that of berberine. It needs to be removed by alcohol precipitation (ethanol concentration of more than 70%), but the alcohol precipitation process will cause 10%-15% of berberine to co-precipitate.
[0006] It is also difficult to remove the pigments in the extract. The phenolic pigments (such as berberine) and tannins (content of about 5%-8%) in the alcohol extract easily form colloids with berberine, resulting in a decrease in the adsorption efficiency of subsequent chromatography columns (such as macroporous resins) and a decrease in column efficiency by 30%-40%.
[0007] For this reason, a Coptidis Rhizoma extraction process is now proposed to solve the above-mentioned problems. Summary of the Invention
[0008] The purpose of the present invention is to provide a Coptidis Rhizoma extraction process to solve the problems raised in the above background technology.
[0009] To achieve the above object, the present invention provides the following technical solution: a process for extracting Coptis chinensis, wherein the specific steps of the process are as follows:
[0010] Step 1: Pretreatment of Coptis chinensis: Select dried Coptis chinensis rhizomes, remove impurities and moldy parts, rinse the treated Coptis chinensis twice with deionized water to remove surface dust, place in a 50-60°C oven to dry until the moisture content is less than 5%, and grind the dried Coptis chinensis through a grinding device. After grinding, pass through an 80-100 mesh sieve to obtain a uniform fine powder;
[0011] Pour the Rhizoma Coptidis powder into a container, add 3-5 times the volume of petroleum ether to the container, stir and degrease at room temperature 2-3 times, each time for 1-2 hours, filter it, and discard the filtrate after filtering;
[0012] Step 2, Coptis chinensis extraction: add 8-10 times the volume of ethanol solution to the defatted Coptis chinensis powder, the concentration of the added ethanol solution is 60-80% (v / v), mix and stir evenly, pour it into an ultrasonic extractor, control the power of the ultrasonic extractor to 300-500W, the temperature to 50-60°C, extract 2-3 times, each time for 30-45 minutes, centrifuge, and collect the supernatant;
[0013] Step 3: Remove impurities and pigments: Add 0.1-0.3% chitosan solution to the extract, mix and stir for 30 minutes, let it stand for 1-2 hours to allow protein and tannin macromolecular impurities to flocculate and precipitate, and filter to remove the precipitate;
[0014] Select non-polar or weakly polar macroporous resin and pack it into the column;
[0015] After filtering the extract through a 0.45 μm microporous membrane, the sample was loaded at a flow rate of 1-2 BV / h (BV is the resin bed volume) until the color of the effluent became significantly lighter. The column bed was first rinsed with 3-5 BV of deionized water to remove water-soluble small molecular impurities; then eluted with 3-5 BV of ethanol solution with an ethanol concentration of 30-50% (v / v) to remove pigments and impurities. Finally, eluted with 5-8 BV of ethanol with an ethanol concentration of 70-90% (v / v) to collect the eluate containing alkaloids such as berberine;
[0016] If there is a lot of pigment residue, add 0.5-1% (w / v) medicinal activated carbon to the eluate, stir and adsorb at 60°C for 30 minutes, filter while hot, and concentrate the filtrate under reduced pressure until there is no alcohol taste;
[0017] Step 4, concentration: add 10% NaOH solution to the concentrate to adjust the pH to 9-10 to free alkaloids such as berberine, let it stand for 12 hours, collect the precipitate by centrifugation, wash it with a small amount of cold water, dissolve the precipitate with 1% hydrochloric acid, adjust the pH to 5-6, and filter to obtain a refined liquid; use a nanofiltration membrane or a reverse osmosis membrane to perform membrane separation on the refined liquid at a pressure of 0.5-1.0 MPa to remove residual small molecular pigments and polypeptides, and at the same time concentrate the active ingredients to a solid content of 5-10%;
[0018] Step 5. Make a paste: Remove the lumps from the concentrated Coptis chinensis extract to ensure uniform dispersion. Take glycerol and purified water, add them to a beaker, and heat them in a water bath while stirring continuously to 60-70°C; slowly add the concentrated Coptis chinensis extract to the warm glycerol-water solution, stirring while adding until the concentrated Coptis chinensis extract is completely dispersed and there is no particle feeling; weigh 1-2 parts of CMC-Na, first swell it into a slurry with a small amount of cold water, and then add it to the above mixture, and continue stirring for 30 minutes until the system becomes a paste.
[0019] Preferably, in step 2, the boiling range of the petroleum ether selected is 60-90°C.
[0020] Preferably, the ethanol solution used in step 2 contains hydrochloric acid with a concentration of 0.5-1%.
[0021] Preferably, in step 2, the centrifugal speed of the ultrasonic extractor is 3000-4000 rpm, and the centrifugal time is controlled to be 8-10 min.
[0022] Preferably, the non-polar or weakly polar macroporous resin selected in step 3 needs to be pre-soaked in an ethanol solution for 20-24 hours. After soaking, it is washed with water until there is no alcohol smell, and the height to diameter ratio of the resin column is 5:1.
[0023] Preferably, the molecular weight cut-off of the nanofiltration membrane selected in step 4 is 300-500 Da.
[0024] Compared with the prior art, the present invention has the following beneficial effects:
[0025] In this Coptis chinensis extraction process, degreasing pretreatment is used to reduce the interference of fat-soluble impurities and improve the efficiency of subsequent resin adsorption. Decolorization by resin can selectively adsorb pigments and polar impurities, retaining effective ingredients such as alkaloids. Membrane separation technology can accurately remove small molecular impurities, replacing traditional activated carbon adsorption and reducing the loss of effective ingredients. Finally, acid-base precipitation method is used for efficient separation and purification, and water-soluble impurities are simultaneously removed. BRIEF DESCRIPTION OF THE DRAWINGS
[0026] Figure 1 The figure is a flow chart of the preparation steps of the present invention. DETAILED DESCRIPTION
[0027] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.
[0028] See also Figure 1 , the present invention provides a technical solution:
[0029] A Coptidis Rhizoma extraction process, the specific steps of the Coptidis Rhizoma extraction process are as follows:
[0030] Step 1: Pretreatment of Coptis chinensis: Select dried Coptis chinensis rhizomes, remove impurities and moldy parts, rinse the treated Coptis chinensis twice with deionized water to remove surface dust, place in a 50-60°C oven to dry until the moisture content is less than 5%, and grind the dried Coptis chinensis through a grinding device. After grinding, pass through an 80-100 mesh sieve to obtain uniform fine powder to increase the dissolution area of the active ingredient during subsequent extraction;
[0031] Pour the Rhizoma Coptidis powder into a container, add 3-5 times the volume of petroleum ether to the container, stir and degrease at room temperature 2-3 times, each time for 1-2 hours, filter it, and discard the filtrate after filtration to remove impurities such as fat-soluble pigments and waxes, thereby reducing fat-soluble interfering components in the subsequent extract;
[0032] Step 2, Coptis chinensis extraction: add 8-10 times the volume of ethanol solution to the defatted Coptis chinensis powder, the concentration of the added ethanol solution is 60-80% (v / v), mix and stir evenly, pour it into an ultrasonic extractor, control the power of the ultrasonic extractor to 300-500W, the temperature to 50-60°C, extract 2-3 times, each time for 30-45 minutes, centrifuge, and collect the supernatant;
[0033] Step 3: Remove impurities and pigments: Add 0.1-0.3% chitosan solution to the extract, mix and stir for 30 minutes, let it stand for 1-2 hours to allow protein and tannin macromolecular impurities to flocculate and precipitate, and filter to remove the precipitate;
[0034] Select non-polar or weakly polar macroporous resin and pack it into the column;
[0035] After filtering the extract through a 0.45 μm microporous membrane, the sample was loaded at a flow rate of 1-2 BV / h (BV is the resin bed volume) until the color of the effluent became significantly lighter. The column bed was first rinsed with 3-5 BV of deionized water to remove water-soluble small molecular impurities; then eluted with 3-5 BV of ethanol solution with an ethanol concentration of 30-50% (v / v) to remove pigments and impurities. Finally, eluted with 5-8 BV of ethanol with an ethanol concentration of 70-90% (v / v) to collect the eluate containing alkaloids such as berberine;
[0036] If there is a lot of pigment residue, add 0.5-1% (w / v) medicinal activated carbon to the eluate, stir and adsorb at 60°C for 30 minutes, filter while hot, and concentrate the filtrate under reduced pressure until there is no alcohol taste;
[0037] Step 4, concentration: add 10% NaOH solution to the concentrate to adjust the pH to 9-10 to free alkaloids such as berberine, let it stand for 12 hours, collect the precipitate by centrifugation, wash it with a small amount of cold water, dissolve the precipitate with 1% hydrochloric acid, adjust the pH to 5-6, and filter to obtain a refined liquid; use a nanofiltration membrane or a reverse osmosis membrane to perform membrane separation on the refined liquid at a pressure of 0.5-1.0 MPa to remove residual small molecular pigments and polypeptides, and at the same time concentrate the active ingredients to a solid content of 5-10%;
[0038] Step 5. Make a paste: Remove the lumps from the concentrated Coptis chinensis extract to ensure uniform dispersion. Take glycerol and purified water, add them to a beaker, and heat them in a water bath while stirring continuously to 60-70°C; slowly add the concentrated Coptis chinensis extract to the warm glycerol-water solution, stirring while adding until the concentrated Coptis chinensis extract is completely dispersed and there is no particle feeling; weigh 1-2 parts of CMC-Na, first swell it into a slurry with a small amount of cold water, and then add it to the above mixture, and continue stirring for 30 minutes until the system becomes a paste.
[0039] In the step 2, the boiling range of the petroleum ether selected is 60-90°C.
[0040] The ethanol solution used in the step 2 contains hydrochloric acid with a concentration of 0.5-1%.
[0041] In the step 2, the centrifugal speed of the ultrasonic extractor is 3000-4000 rpm, and the centrifugal time is controlled to be 8-10 min.
[0042] The non-polar or weakly polar macroporous resin selected in step 3 needs to be soaked in an ethanol solution for 20-24 hours in advance. After soaking, it is washed with water until there is no alcohol smell, and the height to diameter ratio of the resin column is 5:1.
[0043] The molecular weight cut-off of the nanofiltration membrane selected in step 4 is 300-500Da.
[0044] The role of Coptis chinensis extract in cosmetics:
[0045] Anti-inflammatory and soothing, improving sensitive skin: Berberine and other ingredients in Coptis chinensis extract can inhibit the release of inflammatory factors (such as TNF-α, IL-6), reduce skin inflammatory reactions, and relieve sensitive symptoms such as redness, swelling, and stinging; it is suitable for sensitive skin, acne-prone skin, or skin inflammation caused by external stimuli (such as ultraviolet rays and pollution), and can be used in soothing toners, repair masks and other products.
[0046] Antibacterial and antifungal properties, regulating skin microecology: Coptis chinensis extract has an inhibitory effect on common skin pathogens such as Propionibacterium acnes and Staphylococcus aureus, reducing bacterial growth and improving acne and blackheads caused by bacterial infections. It is often used in acne-removing skin care products (such as essences and gels) to help control acne growth, regulate the balance of skin flora, and prevent recurring acne.
[0047] Antioxidant, delaying skin aging: The flavonoids and polysaccharides in it have antioxidant activity, which can scavenge free radicals (such as DPPH free radicals and superoxide anions), reduce the damage of oxidative stress to skin cells, delay collagen loss, and improve fine lines, dullness and other problems. Adding it to anti-aging creams and essences can help improve skin elasticity and radiance.
[0048] Oil control and astringency, improving oily skin: Coptis chinensis extract can inhibit excessive oil secretion from sebaceous glands, while shrinking pores to keep the skin refreshed. It is suitable for oily and combination skin. It is commonly found in oil-control lotions and emulsions, helping to regulate the skin's water and oil balance and reduce shine.
[0049] Regulate skin metabolism and improve dullness: By promoting skin cell metabolism, accelerating the shedding of waste keratin, and reducing melanin deposition, it brightens skin tone and improves dullness and roughness. It can be used in whitening and spot-removing products, and synergizes with other whitening ingredients (such as vitamin C and arbutin) to enhance the brightening effect.
[0050] Example 1:
[0051] The specific steps of the Coptidis Rhizoma extraction process are as follows:
[0052] Step 1: Pretreatment of Coptis chinensis: Select dried Coptis chinensis rhizomes, remove impurities and moldy parts, rinse the treated Coptis chinensis twice with deionized water to remove surface dust, place in a 50-60°C oven to dry until the moisture content is less than 5%, and grind the dried Coptis chinensis through a grinding device. After grinding, pass through an 80-100 mesh sieve to obtain a uniform fine powder;
[0053] Pour the Rhizoma Coptidis powder into a container, add 3 times the volume of petroleum ether to the container, stir and degrease at room temperature 2-3 times, each time for 1-2 hours, filter it, and discard the filtrate after filtering;
[0054] Step 2, Coptis chinensis extraction: add 8-10 times the volume of ethanol solution to the defatted Coptis chinensis powder, the concentration of the added ethanol solution is 60-80% (v / v), mix and stir evenly, pour it into an ultrasonic extractor, control the power of the ultrasonic extractor to 300-500W, the temperature to 50-60°C, extract 2-3 times, each time for 30-45 minutes, centrifuge, and collect the supernatant;
[0055] Step 3: Remove impurities and pigments: Add 0.1% chitosan solution to the extract, mix and stir for 30 minutes, let it stand for 1-2 hours to allow protein and tannin macromolecular impurities to flocculate and precipitate, and filter to remove the precipitate;
[0056] Select non-polar or weakly polar macroporous resin and pack it into the column;
[0057] After filtering the extract through a 0.45 μm microporous membrane, the sample was loaded at a flow rate of 1-2 BV / h (BV is the resin bed volume) until the color of the effluent became significantly lighter. The column bed was first rinsed with 3-5 BV of deionized water to remove water-soluble small molecular impurities; then eluted with 3-5 BV of ethanol solution with an ethanol concentration of 30-50% (v / v) to remove pigments and impurities. Finally, eluted with 5-8 BV of ethanol with an ethanol concentration of 70-90% (v / v) to collect the eluate containing alkaloids such as berberine;
[0058] If there is a lot of pigment residue, add 0.5% (w / v) medicinal activated carbon to the eluate, stir and adsorb at 60°C for 30 minutes, filter while hot, and concentrate the filtrate under reduced pressure until there is no alcohol taste.
[0059] Step 4, concentration: add 10% NaOH solution to the concentrate to adjust the pH to 9-10 to free alkaloids such as berberine, let it stand for 12 hours, collect the precipitate by centrifugation, wash it with a small amount of cold water, dissolve the precipitate with 1% hydrochloric acid, adjust the pH to 5-6, and filter to obtain a refined liquid; use a nanofiltration membrane or a reverse osmosis membrane to perform membrane separation on the refined liquid at a pressure of 0.5-1.0 MPa to remove residual small molecular pigments and polypeptides, and at the same time concentrate the active ingredients to a solid content of 5-10%;
[0060] Step 5. Make a paste: Remove the lumps from the concentrated Coptis chinensis extract to ensure uniform dispersion. Take glycerol and purified water, add them to a beaker, and heat them in a water bath while stirring continuously to 60-70°C; slowly add the concentrated Coptis chinensis extract to the warm glycerol-water solution, stirring while adding until the concentrated Coptis chinensis extract is completely dispersed and there is no particle feeling; weigh 1-2 parts of CMC-Na, first swell it into a slurry with a small amount of cold water, and then add it to the above mixture, and continue stirring for 30 minutes until the system becomes a paste.
[0061] Example 2:
[0062] The specific steps of the Coptidis Rhizoma extraction process are as follows:
[0063] Step 1: Pretreatment of Coptis chinensis: Select dried Coptis chinensis rhizomes, remove impurities and moldy parts, rinse the treated Coptis chinensis twice with deionized water to remove surface dust, place in a 50-60°C oven to dry until the moisture content is less than 5%, and grind the dried Coptis chinensis through a grinding device. After grinding, pass through an 80-100 mesh sieve to obtain a uniform fine powder;
[0064] Pour the Rhizoma Coptidis powder into a container, add 4 times the volume of petroleum ether to the container, stir and degrease at room temperature 2-3 times, each time for 1-2 hours, filter it, and discard the filtrate after filtering;
[0065] Step 2, Coptis chinensis extraction: add 8-10 times the volume of ethanol solution to the defatted Coptis chinensis powder, the concentration of the added ethanol solution is 60-80% (v / v), mix and stir evenly, pour it into an ultrasonic extractor, control the power of the ultrasonic extractor to 300-500W, the temperature to 50-60°C, extract 2-3 times, each time for 30-45 minutes, centrifuge, and collect the supernatant;
[0066] Step 3: Remove impurities and pigments: Add 0.2% chitosan solution to the extract, mix and stir for 30 minutes, let it stand for 1-2 hours to allow protein and tannin macromolecular impurities to flocculate and precipitate, and filter to remove the precipitate;
[0067] Select non-polar or weakly polar macroporous resin and pack it into the column;
[0068] After filtering the extract through a 0.45 μm microporous membrane, the sample was loaded at a flow rate of 1-2 BV / h (BV is the resin bed volume) until the color of the effluent became significantly lighter. The column bed was first rinsed with 3-5 BV of deionized water to remove water-soluble small molecular impurities; then eluted with 3-5 BV of ethanol solution with an ethanol concentration of 30-50% (v / v) to remove pigments and impurities. Finally, eluted with 5-8 BV of ethanol with an ethanol concentration of 70-90% (v / v) to collect the eluate containing alkaloids such as berberine;
[0069] If there is a lot of pigment residue, add 0.75% (w / v) medicinal activated carbon to the eluate, stir and adsorb at 60°C for 30 minutes, filter while hot, and concentrate the filtrate under reduced pressure until there is no alcohol taste.
[0070] Step 4, concentration: add 10% NaOH solution to the concentrate to adjust the pH to 9-10 to free alkaloids such as berberine, let it stand for 12 hours, collect the precipitate by centrifugation, wash it with a small amount of cold water, dissolve the precipitate with 1% hydrochloric acid, adjust the pH to 5-6, and filter to obtain a refined liquid; use a nanofiltration membrane or a reverse osmosis membrane to perform membrane separation on the refined liquid at a pressure of 0.5-1.0 MPa to remove residual small molecular pigments and polypeptides, and at the same time concentrate the active ingredients to a solid content of 5-10%;
[0071] Step 5: Prepare a paste: Remove the lumps from the concentrated Coptis chinensis extract to ensure uniform dispersion. Take glycerol and purified water, add them to a beaker, and heat them in a water bath while stirring continuously to 60-70°C; slowly add the concentrated Coptis chinensis extract to the warm glycerol-water solution, stirring while adding until the concentrated Coptis chinensis extract is completely dispersed and there is no particle feeling; weigh 1-2 parts of CMC-Na, first swell it into a slurry with a small amount of cold water, then add it to the above mixture, and continue stirring for 30 minutes until the system becomes a paste;
[0072] Example 3:
[0073] The specific steps of the Coptidis Rhizoma extraction process are as follows:
[0074] Step 1: Pretreatment of Coptis chinensis: Select dried Coptis chinensis rhizomes, remove impurities and moldy parts, rinse the treated Coptis chinensis twice with deionized water to remove surface dust, place in a 50-60°C oven to dry until the moisture content is less than 5%, and grind the dried Coptis chinensis through a grinding device. After grinding, pass through an 80-100 mesh sieve to obtain a uniform fine powder;
[0075] Pour the Rhizoma Coptidis powder into a container, add 5 times the volume of petroleum ether to the container, stir and degrease at room temperature 2-3 times, each time for 1-2 hours, filter it, and discard the filtrate after filtering;
[0076] Step 2, Coptis chinensis extraction: add 8-10 times the volume of ethanol solution to the defatted Coptis chinensis powder, the concentration of the added ethanol solution is 60-80% (v / v), mix and stir evenly, pour it into an ultrasonic extractor, control the power of the ultrasonic extractor to 300-500W, the temperature to 50-60°C, extract 2-3 times, each time for 30-45 minutes, centrifuge, and collect the supernatant;
[0077] Step 3: Remove impurities and pigments: Add 0.3% chitosan solution to the extract, mix and stir for 30 minutes, let it stand for 1-2 hours to allow protein and tannin macromolecular impurities to flocculate and precipitate, and filter to remove the precipitate;
[0078] Select non-polar or weakly polar macroporous resin and pack it into the column;
[0079] After filtering the extract through a 0.45 μm microporous membrane, the sample was loaded at a flow rate of 1-2 BV / h (BV is the resin bed volume) until the color of the effluent became significantly lighter. The column bed was first rinsed with 3-5 BV of deionized water to remove water-soluble small molecular impurities; then eluted with 3-5 BV of ethanol solution with an ethanol concentration of 30-50% (v / v) to remove pigments and impurities. Finally, eluted with 5-8 BV of ethanol with an ethanol concentration of 70-90% (v / v) to collect the eluate containing alkaloids such as berberine;
[0080] If there is a lot of pigment residue, add 1% (w / v) medicinal activated carbon to the eluate, stir and adsorb at 60°C for 30 minutes, filter while hot, and concentrate the filtrate under reduced pressure until there is no alcohol taste.
[0081] Step 4, concentration: add 10% NaOH solution to the concentrate to adjust the pH to 9-10 to free alkaloids such as berberine, let it stand for 12 hours, collect the precipitate by centrifugation, wash it with a small amount of cold water, dissolve the precipitate with 1% hydrochloric acid, adjust the pH to 5-6, and filter to obtain a refined liquid; use a nanofiltration membrane or a reverse osmosis membrane to perform membrane separation on the refined liquid at a pressure of 0.5-1.0 MPa to remove residual small molecular pigments and polypeptides, and at the same time concentrate the active ingredients to a solid content of 5-10%;
[0082] Step 5. Make a paste: Remove the lumps from the concentrated Coptis chinensis extract to ensure uniform dispersion. Take glycerol and purified water, add them to a beaker, and heat them in a water bath while stirring continuously to 60-70°C; slowly add the concentrated Coptis chinensis extract to the warm glycerol-water solution, stirring while adding until the concentrated Coptis chinensis extract is completely dispersed and there is no particle feeling; weigh 1-2 parts of CMC-Na, first swell it into a slurry with a small amount of cold water, and then add it to the above mixture, and continue stirring for 30 minutes until the system becomes a paste.
[0083] The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention. For those skilled in the art, it is obvious that the present invention is not limited to the details of the above exemplary embodiments, and the present invention can be implemented in other specific forms without departing from the spirit or basic characteristics of the present invention; therefore, no matter from which point of view, the embodiments should be regarded as exemplary and non-restrictive. The scope of the present invention is limited by the appended claims rather than the above description. Therefore, it is intended that all changes that fall within the meaning and scope of the equivalent elements of the claims are included in the present invention, and any figure signs in the claims should not be regarded as limiting the claims involved.
[0084] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.
Claims
1. A process for extracting Coptis chinensis, characterized in that: The specific steps of the Coptidis Rhizoma extraction process are as follows: Step 1: Pretreatment of Coptis chinensis: Select dried Coptis chinensis rhizomes, remove impurities and moldy parts, rinse the treated Coptis chinensis twice with deionized water to remove surface dust, place in a 50-60°C oven to dry until the moisture content is less than 5%, and grind the dried Coptis chinensis through a grinding device. After grinding, pass through an 80-100 mesh sieve to obtain a uniform fine powder; Pour the Rhizoma Coptidis powder into a container, add 3-5 times the volume of petroleum ether to the container, stir and degrease at room temperature 2-3 times, each time for 1-2 hours, filter it, and discard the filtrate after filtering; Step 2, Coptis chinensis extraction: add 8-10 times the volume of ethanol solution to the defatted Coptis chinensis powder, the concentration of the added ethanol solution is 60-80% (v / v), mix and stir evenly, pour it into an ultrasonic extractor, control the power of the ultrasonic extractor to 300-500W, the temperature to 50-60°C, extract 2-3 times, each time for 30-45 minutes, centrifuge, and collect the supernatant; Step 3: Remove impurities and pigments: Add 0.1-0.3% chitosan solution to the extract, mix and stir for 30 minutes, let it stand for 1-2 hours to allow protein and tannin macromolecular impurities to flocculate and precipitate, and filter to remove the precipitate; Select non-polar or weakly polar macroporous resin and pack it into the column; After filtering the extract through a 0.45 μm microporous membrane, the sample was loaded at a flow rate of 1-2 BV / h (BV is the resin bed volume) until the color of the effluent became significantly lighter. The column bed was first rinsed with 3-5 BV of deionized water to remove water-soluble small molecular impurities; then eluted with 3-5 BV of ethanol solution with an ethanol concentration of 30-50% (v / v) to remove pigments and impurities. Finally, eluted with 5-8 BV of ethanol with an ethanol concentration of 70-90% (v / v) to collect the eluate containing alkaloids such as berberine; If there is a lot of pigment residue, add 0.5-1% (w / v) medicinal activated carbon to the eluate, stir and adsorb at 60°C for 30 minutes, filter while hot, and concentrate the filtrate under reduced pressure until there is no alcohol taste; Step 4, concentration: add 10% NaOH solution to the concentrate to adjust the pH to 9-10 to free alkaloids such as berberine, let it stand for 12 hours, collect the precipitate by centrifugation, wash it with a small amount of cold water, dissolve the precipitate with 1% hydrochloric acid, adjust the pH to 5-6, and filter to obtain a refined liquid; use a nanofiltration membrane or a reverse osmosis membrane to perform membrane separation on the refined liquid at a pressure of 0.5-1.0 MPa to remove residual small molecular pigments and polypeptides, and at the same time concentrate the active ingredients to a solid content of 5-10%; Step 5. Make a paste: Remove the lumps from the concentrated Coptis chinensis extract to ensure uniform dispersion. Take glycerol and purified water, add them to a beaker, and heat them in a water bath while stirring continuously to 60-70°C; slowly add the concentrated Coptis chinensis extract to the warm glycerol-water solution, stirring while adding until the concentrated Coptis chinensis extract is completely dispersed and there is no particle feeling; weigh 1-2 parts of CMC-Na, first swell it into a slurry with a small amount of cold water, and then add it to the above mixture, and continue stirring for 30 minutes until the system becomes a paste.
2. A Coptidis Rhizoma extraction process according to claim 1, characterized in that: In the step 2, the boiling range of the petroleum ether selected is 60-90°C.
3. A Coptidis Rhizoma extraction process according to claim 1, characterized in that: The ethanol solution used in the step 2 contains hydrochloric acid with a concentration of 0.5-1%.
4. A Coptidis Rhizoma extraction process according to claim 1, characterized in that: In the step 2, the centrifugal speed of the ultrasonic extractor is 3000-4000 rpm, and the centrifugal time is controlled to be 8-10 min.
5. The process for extracting Coptidis rhizome according to claim 1, wherein: The non-polar or weakly polar macroporous resin selected in step 3 needs to be soaked in an ethanol solution for 20-24 hours in advance. After soaking, it is washed with water until there is no alcohol smell, and the height to diameter ratio of the resin column is 5:
1.
6. A Coptidis Rhizoma extraction process according to claim 1, characterized in that: The molecular weight cut-off of the nanofiltration membrane selected in step 4 is 300-500Da.
Citation Information
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