CN113827633A - A method for preparing Chinese medicinal nanometer powder - Google Patents
A method for preparing Chinese medicinal nanometer powder Download PDFInfo
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- CN113827633A CN113827633A CN202111239595.2A CN202111239595A CN113827633A CN 113827633 A CN113827633 A CN 113827633A CN 202111239595 A CN202111239595 A CN 202111239595A CN 113827633 A CN113827633 A CN 113827633A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/53—Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
- A61K36/481—Astragalus (milkvetch)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/896—Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
- A61K36/8969—Polygonatum (Solomon's seal)
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- 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
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/42—Proteins; Polypeptides; Degradation products thereof; Derivatives thereof, e.g. albumin, gelatin or zein
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- 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
- A61K9/19—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles lyophilised, i.e. freeze-dried, solutions or dispersions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y5/00—Nanobiotechnology or nanomedicine, e.g. protein engineering or drug delivery
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Abstract
The invention provides a preparation method of Chinese herbal medicine ultrafine powder, in particular to a preparation method of nano-scale powder, and particularly relates to a method for preparing Chinese herbal medicine nano-scale powder by a liquid phase method. The advantages are that: (1) the invention can obtain nano-scale dispersion liquid, and further obtain the composition of the nano Chinese herbal medicine/protein composite material. (2) The preparation process is simple, the reaction is easy to control, the adopted equipment is industrial equipment, the stability is good, and industrialization can be realized.
Description
Technical Field
The invention relates to a method for preparing Chinese herbal medicine ultrafine powder, in particular to a method for preparing nano-scale powder, and particularly relates to a method for preparing Chinese herbal medicine nano-scale powder by a liquid phase method.
Background
The stator and rotor continuous dispersion mixer is one of the mixers with wide application range and high efficiency in the current process industry, can generate higher shearing and energy dissipation rate, has shorter retention time, is suitable for dispersion and mixing of materials with various systems and viscosities, and has good application prospect for rapid and complex reaction. Meanwhile, the dispersion mixer can also realize the effect of liquid dispersion. For example, studies have shown that the rotational speed, the residence time, the concentration of the material and the temperature have a large influence on the dispersion.
The nano-crystallization of Chinese herbal medicines is a hot spot of research and development at present. After the Chinese herbal medicines are nanocrystallized, the advantages are as follows: the surface area exposed in the medium is increased, and the dissolution of the effective components is promoted; the adhesion makes the effective component act on the absorption part for a longer time; the distribution of the effective components in the body is increased; the release, absorption and utilization of the effective components are improved; can effectively improve the solubility and dissolution of the active ingredients. The key technology of Chinese herbal medicine nanocrystallization lies in that Chinese herbal medicines are subjected to dispersion treatment, including methods of solid phase dispersion, liquid phase dispersion and the like. However, the method of using a stator-rotor continuous disperser has not been reported for dispersing Chinese herbal medicines.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, aims to provide a preparation method of Chinese herbal medicine ultrafine powder, particularly relates to a preparation method of nano-scale powder, and particularly relates to a method for preparing Chinese herbal medicine nano-scale powder by using a liquid phase method.
The specific scheme of the invention comprises:
(1) selecting one or more solvents, and making the superfine Chinese medicinal powder into primary dispersion (mass fraction greater than 30%). Under the condition of the combined action of stirring and ultrasonic vibration, aqueous solution (mass concentration of 1-10%) containing surfactant (mass concentration of 1-20%) and cosurfactant is slowly dropped (or sprayed) into the dispersion liquid to form suspension of Chinese herbal medicine particles.
(2) The suspension is continuously fed into a stator-rotor continuous dispersion mixer with multi-stage stator-rotor in operation state, and simultaneously, a certain concentration of protein solution with specific Stokes radius is injected.
(3) The slurry continuously flowing out of the mixer is subjected to post-treatment.
The solvent can be selected from water, alcohols, esters, ketones, liquid acids or bases or other solvents. Wherein the alcohol is selected from monohydric alcohol or polyhydric alcohol, such as one of ethanol, propanol, butanol, ethylene glycol, propylene glycol, and glycerol; examples of the ester include one of ethyl lactate, butyl lactate, ethyl acetate, butyl acetate, and Y-butyrolactone; examples of the ketones include acetone, methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone, and methyl pentanone; examples of the acid or base include acetic acid, hydrochloric acid, and sodium hydroxide; examples of other solvents are pyridine, tetrahydrofuran, and the like.
The Chinese herbal medicine powder is subjected to superfine treatment, and the particle size of the Chinese herbal medicine powder is 1-5 microns.
The surfactant and cosurfactant comprise: anionic surfactants such as sodium lauryl sulfate, sodium dodecylbenzenesulfonate and the like; nonionic surfactants such as octadecyl polyoxyethylene, fatty acid sorbitan, polyoxyethylene, polysorbate, and the like; amphoteric surfactants such as amine carboxylates and quaternary ammonium carboxylates; cationic surfactants such as cetyltrimethylammonium bromide and the like; cosurfactant such as alcohols with medium carbon chain length, such as dodecanol, hexadecanol, etc.
The protein solution with the specific Stokes radius is myosin (Stokes radius 20nm), fibrinogen (Stokes radius), thyroglobulin (Stokes radius 8.5nm), urease: (Stocks radius 6.2nm), porcine immunoglobulin (Stocks radius 5.5nm), bovine serum albumin (Stocks radius 3.5nm), ovalbumin (Stocks radius 2.73nm), trypsin inhibitor (Stocks radius 2.26nm), cytochrome C (Stocks radius 1.7 nm).
The stator-rotor continuous dispersion mixer is composed of a rotor and a stator which are coaxial, the rotor stator is provided with or not provided with stirring fins, the rotating speed of the rotor is 500-3The temperature of the mixer is 20-60 ℃.
The post-treatment comprises one of freeze drying, freeze wall breaking treatment and the like. Wherein the temperature of freezing wall breaking is-60 to-30 ℃.
The invention has the advantages that:
(1) the invention can obtain nano-scale dispersion liquid, and further obtain the composition of the nano Chinese herbal medicine/protein composite material.
(2) The preparation process is simple, the reaction is easy to control, the adopted equipment is industrial equipment, the stability is good, and industrialization can be realized.
Detailed Description
The technical solution of the present invention is further described below by specific examples. The following examples are further illustrative of the present invention and do not limit the scope of the present invention.
Example 1
The powder of Orthosiphon aristatus with particle size of 3 μm is added into water to prepare 40% primary dispersion. Slowly dripping 5% of sodium dodecyl benzene sulfonate and 2% of dodecanol under the combined action of stirring and ultrasonic vibration to form a suspension of Chinese herbal medicine particles. Meanwhile, thyroglobulin with the mass concentration of 40% is prepared. Two liquids are injected into a stator-rotor continuous dispersion mixer simultaneously, the rotating speed of the rotor is 10000 r/min, and the flow range of reactant solution passing through the mixer is 2000m3The mixer temperature was 50 ℃. And (4) after the slurry flows out, carrying out freeze drying to finally obtain the nano-scale composite material of the felwort/thyroglobulin.
The particle size of the composite material was 560 nm.
Example 2
Adding radix astragali powder with particle size of 1 micrometer into water/propanol solvent (volume ratio of 1:1) to obtain 50% primary componentAnd (4) dispersing. Slowly dripping 10% octadecyl polyoxyethylene and 5% cetyl alcohol under the combined action of stirring and ultrasonic vibration to form suspension of Chinese herbal medicine particles. Meanwhile, the pig immunoglobulin with the mass concentration of 50% is prepared. Two kinds of liquid are injected into the stator and rotor continuous dispersion mixer simultaneously, the rotating speed of the rotor is 20000 rpm, and the flow range of reactant solution passing through the mixer is 3000m3The mixer temperature was 40 ℃. And (3) after the slurry flows out, freezing and breaking the wall (-40 ℃), and finally obtaining the nano astragalus/pig immunoglobulin composite material.
The particle size of the composite material was 210 nm.
Example 3
Adding rhizoma Polygonati powder with particle size of 2 μm into water/ethanol solvent (volume ratio of 1:1) to obtain 50% primary dispersion. Slowly adding 5% polysorbate and 5% cetyl alcohol dropwise under the combined action of stirring and ultrasonic vibration to form suspension of Chinese medicinal fine particles. Meanwhile, ovalbumin with the mass concentration of 40% is prepared. Two liquids are injected into a stator-rotor continuous dispersion mixer at the same time, the rotating speed of the rotor is 2000 rpm, and the flow range of reactant solution passing through the mixer is 200m3The mixer temperature was 30 ℃. And (4) after the slurry flows out, carrying out freeze drying to finally obtain the composite material of the nano-modified rhizoma polygonati/egg albumin.
The particle size of the composite material was 815 nm.
Claims (7)
1. A preparation method of Chinese herbal medicine ultrafine powder is characterized in that the preparation method comprises the following steps:
(1) selecting one or more solvents, and making the superfine Chinese medicinal powder into primary dispersion (mass fraction greater than 30%). Under the condition of the combined action of stirring and ultrasonic vibration, aqueous solution (mass concentration of 1-10%) containing surfactant (mass concentration of 1-20%) and cosurfactant is slowly dropped (or sprayed) into the dispersion liquid to form suspension of Chinese herbal medicine particles.
(2) The suspension is continuously fed into a stator-rotor continuous dispersion mixer with multi-stage stator-rotor in operation state, and simultaneously, a certain concentration of protein solution with specific Stokes radius is injected.
(3) The slurry continuously flowing out of the mixer is subjected to post-treatment.
2. The method for preparing Chinese herbal medicine micropowder of claim 1, wherein the solvent is selected from water, alcohols, esters, ketones, liquid acids or bases, or other solvents. Wherein the alcohol is selected from monohydric alcohol or polyhydric alcohol, such as one of ethanol, propanol, butanol, ethylene glycol, propylene glycol, and glycerol; examples of the ester include one of ethyl lactate, butyl lactate, ethyl acetate, butyl acetate, and Y-butyrolactone; examples of the ketones include acetone, methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone, and methyl pentanone; examples of the acid or base include acetic acid, hydrochloric acid, and sodium hydroxide; examples of other solvents are pyridine, tetrahydrofuran, and the like.
3. The method of claim 1, wherein the particle size of the herbal powder is 1-5 μm.
4. The process for preparing superfine powder of Chinese herbal medicine as claimed in claim 1, wherein said surfactant and cosurfactant are: anionic surfactants such as sodium lauryl sulfate, sodium dodecylbenzenesulfonate and the like; nonionic surfactants such as octadecyl polyoxyethylene, fatty acid sorbitan, polyoxyethylene, polysorbate, and the like; amphoteric surfactants such as amine carboxylates and quaternary ammonium carboxylates; cationic surfactants such as cetyltrimethylammonium bromide and the like; cosurfactant such as alcohols with medium carbon chain length, such as dodecanol, hexadecanol, etc.
5. The method of preparing chinese herbal medicine micropowder of claim 1, wherein the protein solution of a specific Stokes radius is myosin (Stokes radius 20nm), fibrinogen (Stokes radius), thyroglobulin (Stokes radius 8.5nm), urease: (Stocks radius 6.2nm), porcine immunoglobulin (Stocks radius 5.5nm), bovine serum albumin (Stocks radius 3.5nm), ovalbumin (Stocks radius 2.73nm), trypsin inhibitor (Stocks radius 2.26nm), cytochrome C (Stocks radius 1.7 nm).
6. The method as claimed in claim 1, wherein the stator-rotor continuous dispersion mixer comprises a rotor and a stator which are coaxial, the rotor and the stator are provided or not provided with stirring fins, the rotor speed is 500-3The temperature of the mixer is 20-60 ℃.
7. A method for preparing a Chinese herbal medicine micropowder according to claim 1, wherein said post-treatment comprises one of freeze-drying, freeze-breaking treatment and the like. Wherein the temperature of freezing wall breaking is-60 to-30 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111239595.2A CN113827633A (en) | 2021-10-25 | 2021-10-25 | A method for preparing Chinese medicinal nanometer powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111239595.2A CN113827633A (en) | 2021-10-25 | 2021-10-25 | A method for preparing Chinese medicinal nanometer powder |
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| Publication Number | Publication Date |
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| CN113827633A true CN113827633A (en) | 2021-12-24 |
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| CN202111239595.2A Pending CN113827633A (en) | 2021-10-25 | 2021-10-25 | A method for preparing Chinese medicinal nanometer powder |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5051406A (en) * | 1987-03-04 | 1991-09-24 | Nippon Hypox Laboratories Incorporated | Pharmaceutical composition using albumin as a carrier and process for producing the same |
| WO2003037359A1 (en) * | 2001-10-29 | 2003-05-08 | Chengdu Somo Namotechnology Co., Ltd. | Nanoparticle of insoluble medicinal components and method to produce thereof |
| CN110960602A (en) * | 2019-12-20 | 2020-04-07 | 上海健康医学院 | Method for extracting and nanocrystallizing insoluble components in plant |
| CN111455563A (en) * | 2020-04-20 | 2020-07-28 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of Chinese herbal medicine nanofiber membrane with potential antiviral effect |
-
2021
- 2021-10-25 CN CN202111239595.2A patent/CN113827633A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5051406A (en) * | 1987-03-04 | 1991-09-24 | Nippon Hypox Laboratories Incorporated | Pharmaceutical composition using albumin as a carrier and process for producing the same |
| WO2003037359A1 (en) * | 2001-10-29 | 2003-05-08 | Chengdu Somo Namotechnology Co., Ltd. | Nanoparticle of insoluble medicinal components and method to produce thereof |
| CN110960602A (en) * | 2019-12-20 | 2020-04-07 | 上海健康医学院 | Method for extracting and nanocrystallizing insoluble components in plant |
| CN111455563A (en) * | 2020-04-20 | 2020-07-28 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of Chinese herbal medicine nanofiber membrane with potential antiviral effect |
Non-Patent Citations (2)
| Title |
|---|
| 廖启江，等: "高剪切混合器研究与应用进展", 《化工进展》 * |
| 杨蕾等: "多级定转子连续分散混合器内的微观混合性能", 《北京化工大学学报(自然科学版)》 * |
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