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CN113827633A - A method for preparing Chinese medicinal nanometer powder - Google Patents

A method for preparing Chinese medicinal nanometer powder Download PDF

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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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chinese herbal
herbal medicine
radius
preparation
stocks
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严辰玥
袁艳萍
朱君
罗超
李伟
黄钢
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Shanghai University of Medicine and Health Sciences
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Shanghai University of Medicine and Health Sciences
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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
    • 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)
    • 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)
    • 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
    • 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
    • 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
    • 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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  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Pharmacology & Pharmacy (AREA)
  • General Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
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  • Animal Behavior & Ethology (AREA)
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  • Nanotechnology (AREA)
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  • Bioinformatics & Cheminformatics (AREA)
  • Biophysics (AREA)
  • Molecular Biology (AREA)
  • General Engineering & Computer Science (AREA)
  • Proteomics, Peptides & Aminoacids (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Medicinal Preparation (AREA)

Abstract

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 nanometer powder, in particular to a method for preparing nanometer powder of Chinese herbal medicine by a liquid phase method. device. The advantages are: (1) The present invention can obtain nano-scale dispersion liquid, and then obtain the composite material composition of nano-sized Chinese herbal medicine/protein. (2) The preparation process of the present invention is simple, the reaction is easy to control, and the equipment used is industrialized equipment, which has good stability and can be industrialized.

Description

A method for preparing Chinese medicinal nanometer powder
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)

1.一种中草药超细粉末的制备方法，其特征在于所述的制备方法：1. a preparation method of Chinese herbal medicine ultrafine powder, is characterized in that described preparation method: (1)选择一种或多种溶剂，将超细后中草药粉体制成初级分散液(质量分数大于30％)。在搅拌与超声振动共同作用的条件下，将含表面活性剂(质量浓度为1-20％)和助表面活性剂的水溶液(质量浓度为1-10％)緩慢滴加入(或喷雾加入)分散液中，即形成中草药微粒的悬浮液。(1) One or more solvents are selected, and the superfine Chinese herbal medicine powder is made into a primary dispersion (mass fraction is greater than 30%). Under the condition of stirring and ultrasonic vibration, the aqueous solution containing surfactant (mass concentration of 1-20%) and co-surfactant (mass concentration of 1-10%) is slowly added dropwise (or sprayed) to disperse In the liquid, a suspension of Chinese herbal medicine particles is formed. (2)将上述悬浮液连续送入具有多级定转子的处于运转状态的定转子连续分散混合器中，同时注入一定浓度的特定Stokes半径的蛋白溶液。(2) The above-mentioned suspension is continuously fed into a stator-rotor continuous dispersing mixer with multi-stage stator-rotor in operation state, and a certain concentration of protein solution with a specific Stokes radius is injected at the same time. (3)将从混合器连续流出的浆料进行后处理。(3) Post-treatment of the slurry continuously flowing from the mixer. 2.根据权利要求1所述的一种中草药超细粉末的制备方法，其特征在于所述的溶剂可选自水、醇类、酯类、酮类、液状的酸或碱或其它溶剂。其中醇类选自一元醇或多元醇，如乙醇、丙醇、丁醇、乙二醇、丙二醇、丙三醇等的一种；酯类举例有乳酸乙酯、乳酸丁酯、醋酸乙酯、醋酸丁酯、Y-丁酸内酯等的一种；酮类举例有丙酮、甲乙酮、甲基异丁基酮、环已酮、甲戊酮等的一种；酸或碱类举例有醋酸、盐酸和氢氧化钠等；其它溶剂举例有吡啶、四氢呋喃等的一种。2. The preparation method of a Chinese herbal medicine superfine powder according to claim 1, wherein the solvent can be selected from water, alcohols, esters, ketones, liquid acids or bases or other solvents. Wherein alcohols are selected from monohydric alcohols or polyhydric alcohols, such as one of ethanol, propanol, butanol, ethylene glycol, propylene glycol, glycerol, etc.; esters are exemplified by ethyl lactate, butyl lactate, ethyl acetate, A kind of butyl acetate, gamma-butyric acid lactone, etc.; ketones include a kind of acetone, methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone, methyl amyl ketone, etc.; acids or bases include acetic acid, Hydrochloric acid, sodium hydroxide, etc.; other solvents include pyridine, tetrahydrofuran and the like. 3.根据权利要求1所述的一种中草药超细粉末的制备方法，其特征在于所述的中草药粉体要进行超细处理，其粒径为1-5微米。3. The preparation method of a kind of Chinese herbal medicine ultrafine powder according to claim 1, it is characterized in that described Chinese herbal medicine powder is to carry out ultrafine treatment, and its particle diameter is 1-5 microns. 4.根据权利要求1所述的一种中草药超细粉末的制备方法，其特征在于所述的表面活性剂及助表面活性剂有：阴离子型表面活性剂，如十二烷基硫酸钠，十二烷基笨磺酸钠等；非离子型表面活性剂，如十八烷基聚氧乙烯，脂肪酸失水山梨醇，聚氧乙烯和聚山梨酸酯等；两性表面活性剂，如胺类羧酸盐和季铵盐羧酸盐等；阳离子型表面活性剂，如十六烷基三甲基溴化铵等；助表面活性剂，如中等碳链长度的醇类，如十二醇，十六醇等的一种。4. the preparation method of a kind of Chinese herbal medicine superfine powder according to claim 1 is characterized in that described surfactant and cosurfactant are: anionic surfactant, such as sodium lauryl sulfate, ten Sodium dialkylbenzene sulfonate, etc.; nonionic surfactants, such as octadecyl polyoxyethylene, fatty acid sorbitan, polyoxyethylene and polysorbate, etc.; amphoteric surfactants, such as amine carboxylate acid salts and quaternary ammonium carboxylates, etc.; cationic surfactants, such as cetyltrimethylammonium bromide, etc.; co-surfactants, such as alcohols with medium carbon chain length, such as dodecyl alcohol, ten A kind of hexaol, etc. 5.根据权利要求1所述的一种中草药超细粉末的制备方法，其特征在于所述的特定Stokes半径的蛋白溶液为肌球蛋白(Stokes半径20nm)，纤维蛋白原(Stokes半径)，甲状腺球蛋白(Stocks半径8.5nm)，脲酶：(Stocks半径6.2nm)，猪免疫球蛋白(Stocks半径5.5nm)，牛血清白蛋白(Stocks半径3.5nm)，卵清蛋白(Stocks半径2.73nm)，胰蛋白酶抑制剂(Stocks半径2.26nm)，细胞色素C(Stocks半径1.7nm)的一种。5. the preparation method of a kind of Chinese herbal medicine superfine powder according to claim 1, is characterized in that the protein solution of described specific Stokes radius is myosin (Stokes radius 20nm), fibrinogen (Stokes radius), thyroid Globulin (Stocks 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), a kind of cytochrome C (Stocks radius 1.7nm). 6.根据权利要求1所述的一种中草药超细粉末的制备方法，其特征在于所述的定转子连续分散混合器由同轴的一个转子和一个定子构成，转子定子上设有或者未设有搅拌翅，转子转速为500-20000转/分，反应物溶液通过混合器的流量范围为0.02-3000m3/h，混合器的温度为20-60℃。6. The preparation method of a kind of Chinese herbal medicine superfine powder according to claim 1, it is characterized in that the described stator-rotor continuous dispersing mixer is composed of a coaxial rotor and a stator, and the rotor stator is provided with or not provided with There are stirring fins, the rotor speed is 500-20000 rpm, the flow rate of the reactant solution passing through the mixer is 0.02-3000 m 3 /h, and the temperature of the mixer is 20-60°C. 7.根据权利要求1所述的一种中草药超细粉末的制备方法，其特征在于所述的后处理包含冷冻干燥、冷冻破壁处理等的一种。其中，冷冻破壁的温度为-60～-30℃。7. the preparation method of a kind of Chinese herbal medicine ultrafine powder according to claim 1, is characterized in that described post-processing comprises a kind of freeze-drying, freeze-breaking wall processing etc.. Among them, the temperature of freezing broken wall is -60～-30 ℃.
CN202111239595.2A 2021-10-25 2021-10-25 A method for preparing Chinese medicinal nanometer powder Pending CN113827633A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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CN110960602A (en) * 2019-12-20 2020-04-07 上海健康医学院 Extraction and Nanometerization of Insoluble Components in Plants
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
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 Extraction and Nanometerization of Insoluble Components in Plants
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)

* Cited by examiner, † Cited by third party
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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Application publication date: 20211224