Microencapsulation technology of multi-component Chinese herbal medicine extract

Abstract

The invention discloses a microencapsulation technology of a multi-component Chinese herbal medicine extract, and relates to the technical field of traditional Chinese medicine, and the microencapsulation technology comprises the following steps: S1, cooking Chinese herbal medicine formula powder in an ethanol-water system solvent at high temperature and high pressure, and filtering to remove dregs to obtain a Chinese herbal medicine extracting solution; s2, putting the silicon oxide hollow spheres into the Chinese herbal medicine extracting solution, adding a pH response amphiphilic auxiliary agent, and stirring for 0.5-1 hour; then adjusting the pH value of the Chinese herbal medicine extracting solution to be weakly acidic, and stirring for 0.8-1.2 hours to obtain a weakly acidic extracting solution; and S3, dropwise adding a sodium silicate solution into the weakly acidic extracting solution, heating and stirring until the reaction is complete and microcapsules are formed, filtering to obtain a filter cake, and drying the filter cake to obtain the Chinese herbal medicine extract microcapsules. Different from a traditional water-in-oil or oil-in-water microencapsulation technology, the prepared microcapsule is high in drug effect and high in slow release property, and the preparation method is simple, convenient to apply and capable of being widely applied to the fields of textiles, cosmetics, health care products and the like.

Description

Technical Field

[0001] The present invention relates to the technical field of traditional Chinese medicine, in particular to a microencapsulation technology for multi-component Chinese herbal medicine extracts. Background Art

[0002] In the practical application of Chinese herbal medicine, the combination of different medicinal materials creates a myriad of formulas. Based on the physical and chemical properties of various chemical components in Chinese herbal medicines, over a dozen major categories have been identified, including sugars and glycosides, anthraquinones, phenylpropanoids, flavonoids, tannins, terpenes and volatile oils, steroids, saponins, alkaloids, and organic acids. However, traditional dosage forms and their preparation processes suffer from numerous drawbacks, including low active ingredient concentrations, high dosages, slow onset of action, and the mixing of active ingredients with impurities. Advances in Chinese herbal medicine extraction and separation technologies have led to the emergence of new dosage forms such as tablets, granules, capsules, and film-forming formulations.

[0003] The extract obtained after solvent dissolution extraction has a large volume and low concentration. In addition, many types of active ingredients in Chinese herbal medicine extracts, such as monoterpenes, sesquiterpenes, anthraquinones, baicalin and other compounds, are volatile or heat-sensitive. Therefore, during the actual production, storage and use process, the volatility / sublimation / reducibility of the active ingredients in the Chinese herbal medicine will cause the concentration of the active ingredients in the Chinese herbal medicine to decrease or deteriorate.

[0004] Microencapsulation technology is a technology that uses film-forming materials to encapsulate liquids or solids with reactivity, sensitivity or volatility to form tiny particles. Although this technology has been widely used in the fields of food, pesticides, cosmetics, etc., its application in Chinese herbal medicine preparations has only begun in the 21st century. From the perspective of the principles of microcapsule preparation technology, the technologies suitable for the preparation of Chinese herbal medicine microcapsule preparations mainly include: spray drying, complex coacervation, interfacial polymerization and other physical and chemical methods. For preparations of purified Chinese herbal medicines, the above methods all use a single water or oil phase coating, and cannot simultaneously coat aqueous and oily components. Therefore, it is impossible to completely coat the extracts of Chinese herbal medicine prescriptions, which will cause the effective ingredients to be lost, reducing or even losing their efficacy. The present invention proposes to first enrich the complex water and oily effective ingredients of Chinese herbal medicines by adsorption through hollow microspheres, and then complete the coating by microencapsulation, thereby ensuring the high efficacy of Chinese herbal medicines while facilitating their application. Summary of the Invention

[0005] The purpose of the present invention is to overcome the deficiencies of the prior art and provide a microencapsulation technology for multi-component Chinese herbal medicine extracts, which can completely encapsulate the complex components in the Chinese herbal medicines.

[0006] To achieve the above object, the technical solution adopted by the present invention is as follows:

[0007] A microencapsulation technology for multi-component Chinese herbal medicine extracts, comprising:

[0008] S1: steaming the Chinese herbal formula powder in an ethanol-water solvent system at high temperature and high pressure, filtering and removing the residue to obtain the Chinese herbal extract;

[0009] S2: adding the hollow silica spheres to the Chinese herbal medicine extract, adding a pH-responsive amphiphilic additive, and stirring for 0.5-1 hour; then adjusting the pH value of the Chinese herbal medicine extract to weak acidity and stirring for 0.8-1.2 hours to obtain a weak acidic extract;

[0010] S3: adding sodium silicate solution dropwise to the weakly acidic extract, heating and stirring until the reaction is complete to form microcapsules, filtering to obtain a filter cake, and drying the filter cake to obtain Chinese herbal medicine extract microcapsules.

[0011] Furthermore, the Chinese herbal medicine formula in step S1 includes multiple Chinese herbal medicines, the ethanol content in the ethanol-water system solvent is 5-30%, the cooking temperature is 80-120° C., and the cooking time is 5-8 hours.

[0012] Furthermore, in step S2, the particle size of the hollow silica spheres is 200-800 nm, and the porosity is above 80%; and the amount of the hollow silica spheres added is 1-3% of the mass of the Chinese herbal medicine extract.

[0013] Furthermore, the pH-responsive amphiphilic auxiliary agent in step S2 is of amino acid type.

[0014] Furthermore, the pH-responsive amphiphilic auxiliary agent is an N-alkyl amino acid.

[0015] Furthermore, the amount of sodium silicate solution added in step S3 is 20-60% of the mass of the nano-scale hollow silicon oxide spheres.

[0016] Furthermore, in step S2, the pH value of the Chinese herbal medicine extract is adjusted with citric acid or acetic acid, and the pH value of the weakly acidic extract is 4-6.

[0017] Furthermore, in step S3, the temperature is heated to 30-60°C, the stirring speed is 200-600 r / min, and the reaction time is 1-10 h; and the filter cake is dried at a temperature of 50-80°C.

[0018] Compared with the prior art, the present invention has the following beneficial effects:

[0019] Traditional water-in-oil or oil-in-water microencapsulation technologies can only partially encapsulate Chinese herbal medicine extracts, reducing or even destroying their efficacy. This invention differs from traditional water-in-oil or oil-in-water microencapsulation technologies by utilizing hollow silica to adsorb and enrich various aqueous and oily components of Chinese herbal medicines under different conditions, and then encapsulate them to form microcapsules. This ensures that the vast majority of the active ingredients in the herbal medicines are encapsulated. The resulting microcapsules have high efficacy and strong sustained-release properties. Furthermore, the preparation method is simple and easy to use, making them widely applicable in fields such as textiles, cosmetics, and health products. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 This is a scanning electron microscope image of the Chinese herbal medicine microcapsules prepared in Example 1 of the present invention;

[0021] Figure 2 This is a thermogravimetric analysis chart of the Chinese herbal medicine microcapsules prepared in Example 1 of the present invention;

[0022] Figure 3 This is a graph showing the thermal pyrolysis-mass spectrometry test of the Chinese herbal medicine microcapsules prepared in Example 1 of the present invention;

[0023] Figure 4 This is a scanning electron microscope image of the fabric treated with Chinese herbal medicine microcapsules in an application example of the present invention. DETAILED DESCRIPTION

[0024] The present invention will be further described below with reference to the accompanying drawings and examples. The embodiments of the present invention include but are not limited to the following examples.

[0025] Based on the complexity of Chinese herbal medicine extracts, which contain both aqueous and oily components, this invention proposes using hollow silica microspheres to adsorb the aqueous and oily components separately under the action of amphiphilic additives, and then further encapsulate them into microcapsules. The specific steps include:

[0026] S1: drying, crushing, and grinding a plurality of Chinese herbal medicines to obtain a powder for later use, and then autoclaving the powder in an ethanol-water system at 80-120° C. for 5-8 hours. Filtering and removing residues to obtain a multi-component Chinese herbal extract; wherein the ethanol content in the ethanol-water system is between 5% and 30%;

[0027] S2: Adding 1-3% of nano-sized hollow silica spheres to the extract obtained in step S1, and adding N-alkyl amino acids, stirring for 0.5-1 hour. During this process, the extract is neutral, the amphiphilic excipient exhibits lipophilicity, and most of the oily extract is adsorbed. Further, acid is added to adjust the pH of the extract to a weak acidity (pH of 4-6), and stirring for 0.8-1.2 hours to obtain a weakly acidic extract. At this time, the amphiphilic excipient exhibits hydrophilicity, and most of the aqueous herbal extract is adsorbed.

[0028] The hollow silicon oxide spheres used in this step are nano-scale, with a particle size of 200-800 nm and a porosity of more than 80%;

[0029] S3: Add sodium silicate solution (the addition amount is 20-60% of the nano-scale hollow silica spheres) dropwise into the above-mentioned weakly acidic extract. Under acidic conditions, sodium silicate can be hydrolyzed and condensed to form a silica layer coating on the surface of the hollow silica spheres. Stir at 200-600 r / min at 30-60°C for 1-10 hours until the reaction is complete to form microcapsules; the emulsion after the reaction is filtered and dried at a temperature of 50-80°C to obtain Chinese herbal medicine extract microcapsules.

[0030] Example 1

[0031] In this embodiment, the traditional medicinal pillow formula of Emperor Wu of Han Dynasty is used to prepare microcapsules. The traditional medicinal pillow formula of Emperor Wu of Han Dynasty includes 32 Chinese herbal medicines, namely: white sedge, angelica, Chuanxiong, ginseng, angelica dahurica, dried ginger, gypsum, honeysuckle, chrysanthemum, pepper, privet, asarum, gentian, capillaris, silkworm excrement, cassia seed, vitex negundo seed, white micro, soapwort, wormwood, mint, clove, cinnamon bark, perilla, cyperus rotundus, aconite root, saposhnikovia divaricata, camellia sinensis, Veratrum, Eucommia bark, alum, and winter lily. These 32 Chinese herbal medicines are dried, crushed, mixed, and ground into powder for later use. The method for preparing microcapsules using these 32 Chinese herbal medicines is as follows:

[0032] Add 500 mL of a 10% ethanol solution to 120 g of the powdered formula containing the above 32 Chinese herbal medicines, heat to 80°C with stirring, and steam under pressure in a closed system for 5 h. Then cool to room temperature and filter out the residue for later use.

[0033] 10 g of hollow silica microspheres were added to the above extract, and 0.3 g of N-alkyl amino acid was added. After vigorous stirring for 0.5 h, citric acid was added to adjust the pH to 5. Stirring was continued for 1 h to complete the enrichment and adsorption, and a dark suspension was obtained.

[0034] Dissolve 1g of sodium silicate in 5mL of water and add dropwise to the suspension. Stir at low speed for 8h to complete hydrolysis and polycondensation to obtain an emulsion. Filter the emulsion and dry the filter cake to obtain the Chinese herbal medicine microcapsules.

[0035] The prepared Chinese herbal medicine microcapsules were observed using a German Zeiss ULTRA55 thermal field emission scanning electron microscope. The results are as follows: Figure 1 As shown in Figure 2, the particle size is about 1 μm. The prepared Chinese herbal medicine microcapsules were tested using a PE company Pyris 1 thermogravimetric analyzer. Under nitrogen protection, the temperature was increased from room temperature to 600°C at a rate of 10°C / min, and the weight loss curve was recorded. Figure 2 As shown in the figure, the content of Chinese herbal medicine extract is calculated to be about 40%. The prepared Chinese herbal medicine microcapsules were tested by thermal pyrolysis-mass spectrometry, and the results are as follows Figure 3As shown in the figure, the Chinese herbal medicine components in the microcapsules are basically consistent with the extracts.

[0036] Example 2

[0037] Add 100g of the powder of the traditional Hanwu Emperor medicinal pillow formula to 400mL of a solution containing 15% ethanol, heat to 90°C with stirring, steam under pressure in a closed system for 8h, cool to room temperature, filter out the residue and set aside;

[0038] 5g of hollow silica microspheres were added to the above extract, along with 0.2g of N-alkyl amino acid, and stirred vigorously for 1h. Citric acid was added to adjust the pH to 6, and stirring was continued for 1h to complete enrichment and adsorption, yielding a dark suspension.

[0039] 2 g of sodium silicate was dissolved in 5 mL of water and added dropwise to the suspension. The suspension was stirred at a low speed for 5 h to complete the hydrolysis and polycondensation. The emulsion was filtered and the filter cake was dried to obtain the Chinese herbal medicine extract microcapsules.

[0040] Example 3

[0041] 300g of the powder of the traditional Hanwu Emperor medicinal pillow formula was added to 1500mL of a solution containing 10% ethanol, heated to 95°C with stirring, and pressure-cooked in a closed system for 6h, then cooled to room temperature, and the residue was filtered out for later use;

[0042] 10g of hollow silica microspheres were added to the above extract, along with 0.8g of N-alkyl amino acid, and stirred vigorously for 1h. Citric acid was added to adjust the pH to 5, and stirring was continued for 1h to complete enrichment and adsorption, yielding a dark suspension.

[0043] 8 g of sodium silicate was dissolved in 10 mL of water and added dropwise to the suspension. The suspension was stirred at a low speed for 6 h to complete the hydrolysis and polycondensation. The emulsion was filtered and the filter cake was dried to obtain the Chinese herbal medicine extract microcapsules.

[0044] Application Examples

[0045] The traditional Han Wudi medicinal pillow formula was steamed at high temperature to obtain a multi-component Chinese herbal medicine extract. The Chinese herbal medicine extract was used to prepare the Han Wudi medicinal pillow formula microcapsules. The microcapsules were then treated on cotton fabrics by post-finishing methods (padding, coating or printing) at a content of 10%. The surface morphology of the fabrics was observed under an electron microscope. Figure 4 As shown, a large number of microcapsules were found attached to the fibers.

[0046] The fabric was sewn into pillowcases to create a Han Wudi medicinal pillow. Testing revealed that the pillow had the same efficacy as traditional herbal sachets. The resulting Chinese herbal microcapsules also offer a wider range of applications, including topical applications such as facial masks and creams, demonstrating their exceptional usability. Furthermore, compared to traditional herbal sachets, the fabric sachets exhibit superior sustained-release properties, demonstrating lasting medicinal effects for over two years.

[0047] The above embodiment is only one of the preferred implementation methods of the present invention and should not be used to limit the scope of protection of the present invention. Any changes or modifications that have no substantive meaning made to the main design concept and spirit of the present invention, as long as the technical problems solved are still consistent with the present invention, should be included in the scope of protection of the present invention.

Claims

1. A microencapsulation technology for multi-component Chinese herbal medicine extracts, characterized in that: include: S1: steaming the Chinese herbal formula powder in an ethanol-water solvent system at high temperature and high pressure, filtering and removing the residue to obtain the Chinese herbal extract; S2: adding the hollow silica spheres to the Chinese herbal medicine extract, adding a pH-responsive amphiphilic additive, and stirring for 0.5-1 hour; then adjusting the pH value of the Chinese herbal medicine extract to weak acidity and stirring for 0.8-1.2 hours to obtain a weak acidic extract; S3: adding sodium silicate solution dropwise to the weakly acidic extract, heating and stirring until the reaction is complete to form microcapsules, filtering to obtain a filter cake, and drying the filter cake to obtain Chinese herbal medicine extract microcapsules.

2. The microencapsulation technology of a multi-component Chinese herbal medicine extract according to claim 1, characterized in that: The Chinese herbal medicine formula in step S1 includes multiple Chinese herbal medicines, the ethanol content in the ethanol-water system solvent is 5-30%, the cooking temperature is 80-120° C., and the cooking time is 5-8 hours.

3. The microencapsulation technology of a multi-component Chinese herbal medicine extract according to claim 1, characterized in that: In step S2, the particle size of the hollow silicon oxide spheres is 200-800 nm, and the porosity is above 80%. The amount of the hollow silicon oxide spheres added is 1-3% of the mass of the Chinese herbal medicine extract.

4. The microencapsulation technology of a multi-component Chinese herbal medicine extract according to claim 3, characterized in that: The pH-responsive amphiphilic auxiliary agent in step S2 is of amino acid type.

5. The microencapsulation technology of a multi-component Chinese herbal medicine extract according to claim 4, characterized in that: The pH-responsive amphiphilic adjuvant is an N-alkyl amino acid.

6. The microencapsulation technology of a multi-component Chinese herbal medicine extract according to claim 1, 2 or 5, characterized in that: The amount of sodium silicate solution added in step S3 is 20-60% of the mass of the hollow silicon oxide spheres.

7. The microencapsulation technology of a multi-component Chinese herbal medicine extract according to claim 6, characterized in that: In step S2, the pH value of the Chinese herbal medicine extract is adjusted with citric acid or acetic acid, and the pH value of the weakly acidic extract is 4-6.

8. The microencapsulation technology of a multi-component Chinese herbal medicine extract according to claim 7, characterized in that: In step S3, the mixture is heated to 30-60° C., the stirring speed is 200-600 r / min, and the reaction time is 1-10 h; and the filter cake is dried at a temperature of 50-80° C.

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