CN113456697A - Method for preparing stable polydatin-containing extract and extract thereof - Google Patents

Method for preparing stable polydatin-containing extract and extract thereof Download PDF

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CN113456697A
CN113456697A CN202010238151.6A CN202010238151A CN113456697A CN 113456697 A CN113456697 A CN 113456697A CN 202010238151 A CN202010238151 A CN 202010238151A CN 113456697 A CN113456697 A CN 113456697A
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extract
sodium
polydatin
antioxidant
medicinal materials
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张许科
段飞燕
李焕娟
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Luoyang Huizhong Animal Medicine Co ltd
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Luoyang Huizhong Animal Medicine Co ltd
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    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/02—Inorganic compounds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/08—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing oxygen, e.g. ethers, acetals, ketones, quinones, aldehydes, peroxides
    • A61K47/12—Carboxylic acids; Salts or anhydrides thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/16—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing nitrogen, e.g. nitro-, nitroso-, azo-compounds, nitriles, cyanates
    • A61K47/18—Amines; Amides; Ureas; Quaternary ammonium compounds; Amino acids; Oligopeptides having up to five amino acids
    • A61K47/183—Amino acids, e.g. glycine, EDTA or aspartame
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605—Excipients; Inactive ingredients
    • A61K9/1617—Organic compounds, e.g. phospholipids, fats
    • A61K9/1623—Sugars or sugar alcohols, e.g. lactose; Derivatives thereof; Homeopathic globules
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61P11/00—Drugs for disorders of the respiratory system
    • A61P11/10—Expectorants
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    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P11/00—Drugs for disorders of the respiratory system
    • A61P11/14—Antitussive agents
    • A—HUMAN NECESSITIES
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    • A61P29/00—Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
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    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30—Extraction of the material
    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K2236/30—Extraction of the material
    • A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying

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Abstract

The invention discloses an extraction method capable of improving the stability of polydatin in polygonum cuspidatum. The specific operation is as follows: adding pH regulator and antioxidant into water to extract rhizoma Polygoni Cuspidati powder, wherein the pH regulator comprises hydrochloric acid, acetic acid, sodium hydroxide, sodium carbonate, sodium bicarbonate, and sodium diglycine, and the antioxidant comprises sodium sulfite, sodium thiosulfate, and disodium ethylene diamine tetraacetate. Compared with the single water extraction method, the polydatin is more stable and has higher yield; compared with the organic solvent extraction method, the polydatin has high stability and good water solubility, and the method is safer and more environment-friendly, has strong operability, and is suitable for large-scale industrial production.

Description

Method for preparing stable polydatin-containing extract and extract thereof
Technical Field
The invention belongs to the technical field of extraction of traditional Chinese medicinal materials for livestock, and particularly relates to a method for preparing an extract containing stable polydatin and the extract.
Background
Giant knotweed rhizome is the dried rhizome and root of giant knotweed rhizome in Polygonaceae, has the effects of promoting blood circulation, relieving pain, dispelling wind, promoting diuresis, relieving cough, reducing phlegm, clearing heat and removing toxicity, and belongs to one of widely applied veterinary medicines. Polydatin is one of the effective components of rhizoma Polygoni Cuspidati, and belongs to stilbene compounds.
The polydatin component is reported to be unstable to photo-heat in the literature, but no improvement solution is available. Through experiments, the following results are found: the extraction rate of polydatin is low by only using water as a solvent to extract the giant knotweed rhizome; the polygonum cuspidatum is extracted by using an organic solvent, the water solubility of the polydatin is poor, the risk of blocking a drinking water line exists, and the requirement of drinking water line administration cannot be met.
Therefore, it is desirable to provide a method for extracting polydatin, which can ensure the stability of polydatin in the extract and increase the water solubility of polydatin.
Disclosure of Invention
The invention provides an extraction method capable of improving the stability of polydatin in polygonum cuspidatum. The method disclosed by the invention can improve the stability and water solubility of the polydatin component, is safe and environment-friendly, has strong operability, and is suitable for large-scale industrial production.
The invention provides a method for preparing a stable polydatin-containing extract, which comprises the following steps: adding a pH regulator and an antioxidant into water, and regulating the pH of the solution to 6-8 to prepare a solution A; the dosage of the antioxidant is 0.1 w/w% -1 w/w% of the total weight of the medicinal materials, and the medicinal materials are giant knotweed or compound Chinese medicinal materials containing giant knotweed; and (2) crushing the giant knotweed into coarse powder, and soaking and extracting the solution A in the step (1).
The antioxidant is used in an amount selected from 0.1 w/w%, 0.2 w/w%, 0.3 w/w%, 0.4 w/w%, 0.5 w/w%, 0.6 w/w%, 0.7 w/w%, 0.8 w/w%, 0.9 w/w%, 1 w/w% of the total weight of the medicinal materials.
As an embodiment of the present invention, in the step (1), the pH regulator is one or more of hydrochloric acid, acetic acid, sodium hydroxide, sodium bicarbonate, sodium carbonate, and sodium diglycine carbonate; the antioxidant is one or more of sodium sulfite, sodium thiosulfate and ethylene diamine tetraacetic acid.
As an embodiment of the invention, the compound traditional Chinese medicinal materials containing polygonum cuspidatum in the step (1) comprise 100-500 parts of dandelion, 100-500 parts of polygonum cuspidatum, 100-500 parts of patrinia scabiosaefolia link and 50-250 parts of sculellaria barbata.
As an embodiment of the invention, in the step (2), the solid-to-liquid ratio is 1:6-1:10, the soaking time is 30-60min, the extraction time is 1-2h, and the extraction times are 2-3.
The solid-liquid ratio in the step (2) is 1:6, 1:7, 1:8, 1:9 and 1: 10.
As an implementation manner of the present invention, the step (2) further includes an extraction process of other traditional Chinese medicinal materials in the compound traditional Chinese medicinal material containing polygonum cuspidatum.
As an embodiment of the present invention, the step (2) further includes a preparation process of the formulation.
The invention also provides the extract prepared by the method.
As an embodiment of the present invention, the extract preparation is a granule.
The invention has the beneficial effects that:
(1) the invention aims to improve the stability and the solubility of the polydatin by adding a pH regulator and an antioxidant into an extraction solvent. The stability of the composition is improved through the co-extraction process of the pH regulator, the antioxidant and the medicinal materials;
(2) the extraction method disclosed by the invention is safe and environment-friendly, low in production cost, strong in production operability and suitable for large-scale industrial production.
Detailed Description
The invention will be further described with reference to specific embodiments, and the advantages and features of the invention will become apparent as the description proceeds. These examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention.
The chemical reagents used in the examples of the present invention are all analytical reagents and purchased from the national pharmaceutical group. The experimental methods are conventional methods unless specified otherwise; the biomaterial is commercially available unless otherwise specified.
Example 1 extraction of Polydatin extract and content analysis according to the method of the invention and conventional methods
1.1 the method of the invention extracts the polydatin extract
(1) Adding a proper amount of sodium carbonate into 600ml of water, and adjusting the pH value to 7.5; then adding 0.5g of disodium ethylene diamine tetraacetate, and stirring to dissolve;
(2) pulverizing rhizoma Polygoni Cuspidati into coarse powder, collecting 100g, adding into the solution of step (1), soaking for 30min, extracting for 2 times, each for 1 h;
(3) mixing filtrates, concentrating under reduced pressure, drying, and pulverizing to obtain rhizoma Polygoni Cuspidati extract powder.
1.2 comparative example 1 extraction of Polydatin extract by conventional Water extraction method
Soaking 100g rhizoma Polygoni Cuspidati coarse powder in 600ml water for 30min, extracting for 2 times, each for 1 hr, mixing filtrates, concentrating under reduced pressure, drying, and pulverizing to obtain rhizoma Polygoni Cuspidati extract powder.
1.3 comparative example 2 extraction of Polydatin extract by conventional alcohol extraction method
Soaking 100g rhizoma Polygoni Cuspidati coarse powder in 600ml 70% ethanol solution for 30min, extracting for 2 times, each for 1 hr, mixing filtrates, concentrating under reduced pressure, drying, and pulverizing to obtain rhizoma Polygoni Cuspidati extract powder.
The results are shown in Table 1.
TABLE 1
Figure BDA0002431698910000031
Note: the water solubility test is carried out by weighing 0.5g of extract powder, adding 100ml of hot water, and observing.
The results in table 1 show that:
(1) the invention can improve the stability and yield of polydatin in giant knotweed and compound preparations containing giant knotweed;
(2) the invention can improve the water-dissolving performance of the polydatin.
Example 2 preparation of Compound Chinese medicinal granule containing Polygonum cuspidatum
2.1 the method of the invention extracts the compound traditional Chinese medicine polydatin extract
The method comprises the following steps:
(1) weighing 100-500 parts of dandelion, 100-500 parts of polygonum cuspidatum, 100-500 parts of patrinia scabiosaefolia and 50-250 parts of sculellaria barbata, wherein 285.7g of dandelion, 285.7g of polygonum cuspidatum, 285.7g of patrinia scabiosaefolia and 142.8g of sculellaria barbata are weighed in the embodiment;
(2) pulverizing rhizoma Polygoni Cuspidati into coarse powder;
(3) adding a pH regulator and an antioxidant into water 6-8 times of the weight of the medicinal materials to prepare a solution A; in this embodiment, 7g of sodium hydroxide and 1.5g of sodium thiosulfate are added to 8L of water to obtain a solution A;
(4) putting the whole formula of medicinal materials into an extraction device, adding the solution A obtained in the step (3), soaking for 30-60min, and extracting for 2-3 times, wherein each time for 1-2 h; in this example, soaking for 30min, extracting for 3 times, each time for 1h, filtering, and combining all filtrates;
(5) concentrating the liquid medicine obtained in the step (4) under reduced pressure to obtain an extract with a relative density of 1.0-1.2(70 ℃), centrifuging to obtain a supernatant, wherein the centrifugation parameter range is 8000-; in this example, the liquid medicine is concentrated to a relative density of 1.1(70 ℃), and centrifuged at 8000r/min for 20 min;
(6) concentrating the centrifugal supernatant obtained in the step (5) under reduced pressure until the relative density is 1.2-1.5(70 ℃); in this example, the supernatant liquid was concentrated to a clear paste with a relative density of 1.2(70 ℃);
(7) taking the extract obtained in the step (6) as an adhesive, adding auxiliary materials including sucrose, dextrin, lactose and mannitol, and preparing into granules; in the embodiment, the auxiliary material is sucrose, and 1000g of granules are prepared.
2.2 comparative example 2 extraction of compound traditional Chinese medicine polydatin extract by traditional method
(1) Weighing 285.7g of dandelion, 285.7g of giant knotweed rhizome, 285.7g of patrinia scabiosaefolia and 142.8g of barbed skullcap herb
(2) Pulverizing rhizoma Polygoni Cuspidati into coarse powder;
(3) placing the above materials in an extraction device, adding 8L water, soaking for 30min, extracting for three times, each time for 1 hr, filtering, and mixing all filtrates;
(4) concentrating the liquid medicine obtained in the step (4) under reduced pressure to relative density of 1.1(70 ℃), and centrifuging, wherein the centrifugation parameters are as follows: rotating at 8000r/min, centrifuging for 20 min;
(5) concentrating the centrifugate obtained in the step (5) under reduced pressure to obtain fluid extract with relative density of 1.2(70 deg.C);
(6) and (4) taking the extract obtained in the step (6) as an adhesive, adding cane sugar, and preparing into 1000g of granules.
The test results are shown in Table 2.
TABLE 2
Figure BDA0002431698910000051
The results in table 2 show that:
(1) the invention can improve the stability and extraction rate of polydatin in giant knotweed rhizome and compound preparations containing the same;
(2) the invention can improve the water-dissolving performance of the polydatin.
And (4) conclusion: compared with the extract extracted by the traditional process, the preparation process has higher content of effective components, higher stability and better water solubility; according to the invention, the pH regulator, the antioxidant and the medicinal materials are added into the solvent for co-extraction, so that the stability of the polydatin is improved, the water-soluble property of the finished product in the compound preparation can be improved, and the actual application requirements of veterinary medicines are met. The whole process is safe and environment-friendly, and has strong operability and stable product quality.
The above description is only a preferred embodiment of the present invention, and should not be construed as limiting the invention, and any modification, equivalent exchange, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (8)

1. A method for preparing an extract containing stable polydatin, comprising the steps of:
adding a pH regulator and an antioxidant into water, and regulating the pH of the solution to 6-8 to prepare a solution A; the dosage of the antioxidant is 0.1 w/w% -1 w/w% of the total weight of the medicinal materials, and the medicinal materials are giant knotweed or compound Chinese medicinal materials containing giant knotweed; and
and (2) crushing the giant knotweed into coarse powder, and soaking and extracting by using the solution A in the step (1).
2. The method according to claim 1, wherein the pH regulator in step (1) is one or more of hydrochloric acid, acetic acid, sodium hydroxide, sodium bicarbonate, sodium carbonate, and sodium diglycine carbonate; the antioxidant is one or more of sodium sulfite, sodium thiosulfate and ethylene diamine tetraacetic acid.
3. The method according to claim 1, wherein the compound Chinese medicinal material containing polygonum cuspidatum in the step (1) comprises 100-500 parts of dandelion, 100-500 parts of polygonum cuspidatum, 100-500 parts of patrinia scabiosaefolia link and 50-250 parts of sculellaria barbata.
4. The method according to claim 1, wherein the solid-to-liquid ratio in the step (2) is 1:6-1:10, the soaking time is 30-60min, the extraction time is 1-2h, and the extraction times are 2-3.
5. The method according to claim 1, wherein the step (2) further comprises an extraction process of other Chinese medicinal materials in the compound Chinese medicinal material containing the giant knotweed rhizome.
6. The method of claim 1, wherein step (2) further comprises a formulation preparation process.
7. An extract prepared according to the method of claims 1-6.
8. The extract as claimed in claim 7, wherein the extract preparation is a granule.
CN202010238151.6A 2020-03-30 2020-03-30 Method for preparing stable polydatin-containing extract and extract thereof Pending CN113456697A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1742791A (en) * 2005-09-30 2006-03-08 吕相刚 Heat-clearing toxifying soft capsule and preparing method
CN102718811A (en) * 2012-05-22 2012-10-10 中国人民解放军第四军医大学 Preparation method of stilbene glycoside in polygonum cuspidatum
CN108440616A (en) * 2018-05-30 2018-08-24 云南海沣药业有限公司 A kind of extraction separation method of polygonin

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1742791A (en) * 2005-09-30 2006-03-08 吕相刚 Heat-clearing toxifying soft capsule and preparing method
CN102718811A (en) * 2012-05-22 2012-10-10 中国人民解放军第四军医大学 Preparation method of stilbene glycoside in polygonum cuspidatum
CN108440616A (en) * 2018-05-30 2018-08-24 云南海沣药业有限公司 A kind of extraction separation method of polygonin

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Application publication date: 20211001