A method for preparing Chinese medicinal nanometer powder
阅读说明：本技术 一种中草药纳米级粉末的制备方法 (A method for preparing Chinese medicinal nanometer powder ) 是由 严辰玥 袁艳萍 朱君 罗超 李伟 黄钢 于 2021-10-25 设计创作，主要内容包括：本发明提供一种中草药超细粉末的制备方法,具体涉及一种纳米级粉末的制备方法,尤其涉及一种利用液相法制备中草药纳米级粉末的方法,该方法的设备为定转子连续分散混合器。其优势在于：(1)本发明能够得到纳米级的分散液,进而得到纳米化中草药/蛋白的复合材料组成。(2)本发明制备过程简单、反应易控制,采用设备为工业化设备,稳定性好、可产业化。(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.)
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 ℃.
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.