Propolis composition and preparation method and device thereof

The preparation process of propolis compositions is optimized through supercritical CO2 extraction and nanoification technology, and the problems of complex preparation and low bioavailability of propolis compositions are solved, and efficient and stable preparation of propolis compositions is achieved, which is suitable for functional foods and dietary supplements.

CN120381482APending Publication Date: 2025-07-29JIANGSU RIGAO BEE PROD
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Patent Information

Application Number
CN202510777775.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-06-11
Publication Date
2025-07-29

AI Technical Summary

Technical Problem

The existing propolis composition preparation process is complex, involving multi-step ethanol extraction and water extraction, high energy consumption and large fluctuations between batches, which limits its industrial application and is low in bioavailability, making it difficult to take into account both food-grade safety and long-term consumption needs.

Method used

The propolis nanodispersion is prepared by using supercritical CO2 extraction combined with nanoification technology, combining the synergistic effects of probiotic powder and astragalus polysaccharide, through enzymatic decoction, ultrasonic decoction, nanodispersion and fluidized bed coating, and the supercritical extraction, dynamic mixing and online detection modules are integrated to optimize the preparation process of propolis composition.

Benefits of technology

It significantly improves the bioavailability of propolis, enhances the intestinal barrier function, reduces production energy consumption, improves the retention rate of active ingredients, ensures the stability and safety of the product, and is suitable for functional foods and dietary supplements.

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Abstract

The invention relates to the technical field of treatment of stomach diseases, and provides a propolis composition which is prepared from the following raw materials in parts by weight: 5-30 parts of propolis, 3-20 parts of radix angelicae sinensis, 3-20 parts of rhizoma chuanxiong, 5-25 parts of paederia scandens and 2-15 parts of rhizoma atractylodis macrocephalae. The auxiliary material comprises at least one of microcrystalline cellulose, hydroxypropyl methyl cellulose and magnesium stearate, and the additive comprises 0.1-2 parts of probiotic powder and 3-10 parts of fructo-oligosaccharide, wherein the auxiliary material accounts for 15-35% of the total weight of the auxiliary material; and carrying materials: 2-12 parts of astragalus membranaceus and 1-8 parts of liquorice. Through the synergistic effect of propolis flavone, astragalus polysaccharide and probiotics, the serum IgG and IgA levels are increased by 30-40%, and the NK cell activity is increased by 45%; the abundance of intestinal lactobacillus / bifidobacterium is increased by 3-4 times, the content of short-chain fatty acid is increased by 50%, and the intestinal barrier function is remarkably enhanced; and the levels of inflammatory factors IL-6 and TNF-alpha are reduced by 30-40%, which is superior to that of a single propolis preparation.
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Description

Technical Field

[0001] The present invention relates to the technical field of treating stomach diseases, and specifically to a preparation method and device of a propolis composition and the propolis composition. Background Art

[0002] As a natural active substance, propolis is rich in flavonoids and phenolic acid compounds, and has antibacterial, antioxidant and immunomodulatory effects. In recent years, it has been widely used in the fields of functional foods and health products. Currently, propolis-related patented technologies mainly focus on the medicinal field: CN100496522C discloses an immune-enhancing composition containing propolis, angelica and ligusticum wallichii, and uses supercritical CO2 to extract volatile oils, but does not solve the problems of the bitterness of propolis and intestinal compatibility; CN100453100C proposes a stomach disease treatment composition containing propolis, and is formulated with traditional Chinese medicines such as coptis chinensis, but the medicinal ingredients may cause safety risks during long-term use; in traditional processes, most propolis preparations use simple alcohol extraction or water extraction, with low retention rates of active ingredients, and do not integrate modern nanotechnology or targeted release technology, resulting in insufficient bioavailability.

[0003] However, a single propolis ingredient has problems such as low bioavailability, bitter taste and poor stability, and traditional compound preparations mainly focus on medicinal functions, making it difficult to balance food-grade safety and long-term use requirements. In addition, the existing preparation process of propolis compositions is complex, involving multiple steps of ethanol extraction and water extraction, with high energy consumption and large quality fluctuations between batches, which limits its industrial application. Summary of the Invention

[0004] Aiming at the deficiencies of the prior art, the present invention provides a preparation method and device of a propolis composition and the propolis composition, and solves the problems that the existing preparation process of propolis compositions is complex, involves multiple steps of ethanol extraction and water extraction, has high energy consumption and large quality fluctuations between batches, which limits its industrial application.

[0005] To achieve the above objectives, the present invention is realized through the following technical solutions: A propolis composition, comprising raw materials composed of the following parts by weight:

[0006] 5-30 parts of propolis, 3-20 parts of angelica, 3-20 parts of ligusticum wallichii, 5-25 parts of paederia scandens, 2-15 parts of atractylodes macrocephala;

[0007] Excipients: at least one of microcrystalline cellulose, hydroxypropyl methylcellulose, magnesium stearate, and the total weight ratio of the excipients is 15-35%

[0008] Additives: 0.1-2 parts of probiotic powder, 3-10 parts of fructooligosaccharide;

[0009] Carriers: 2-12 parts of astragalus membranaceus, 1-8 parts of licorice.

[0010] Preferably, the specific weight ratio of the raw materials is as follows:

[0011] 15 parts of propolis, 10 parts of angelica, 8 parts of chuanxiong, 12 parts of paederia scandens, 6 parts of atractylodes macrocephala, 5 parts of astragalus membranaceus, 3 parts of licorice, 0.5 part of probiotic powder, and 6 parts of fructooligosaccharide.

[0012] Preferably, the propolis is Brazilian green propolis with a total flavonoid content ≥ 20%, and is treated by supercritical CO2 dewaxing with a wax residue content ≤ 0.5%.

[0013] Preferably, the viable count of the probiotic powder ≥ 1×10^10 CFU / g, and is treated by microencapsulation. The probiotic powder is any one of the genus Lactobacillus or Bifidobacterium.

[0014] A preparation method of a propolis composition includes the following steps:

[0015] Step 1: Crush angelica, chuanxiong, and paederia scandens to 40 - 60 mesh, add a citric acid buffer solution with a pH of 4.5 - 5.5 according to a solid - liquid ratio of 1:8 - 12, add 0.5 - 1.5 wt% of a composite enzyme, enzymolyze at 45 - 55 °C for 1 - 2 hours, and inactivate after enzymolysis;

[0016] Step 2: Extract the enzymolyzed angelica and chuanxiong by supercritical CO2 with a pressure of 25 - 35 MPa, a temperature of 35 - 45 °C, an entrainer of ethanol with a flow rate of 0.5 - 1.5 mL / min, and an extraction time of 3 - 5 hours to collect the volatile oil. Additionally, mix the extraction residue with paederia scandens and atractylodes macrocephala, add 8 - 10 times the amount of water, and decoct twice under ultrasonic assistance at a frequency of 40 kHz and a power of 300 W for 1 hour each time, and combine the decoction liquids;

[0017] Step 3: Mix propolis and polyvinylpyrrolidone according to a mass ratio of 1:0.3 - 0.6, dissolve in an ethanol - aqueous solution, and circulate and process with a high - pressure homogenizer at 150 - 200 MPa for 3 - 5 times to obtain a propolis nano - dispersion with a particle size ≤ 200 nm;

[0018] Step 4: Add ethanol to the decoction liquid in Step 2 until the alcohol content is 30%, let it stand for 6 hours and then take the supernatant; continue to add ethanol until the alcohol content is 70%, let it stand for 12 hours, and take the precipitate; combine the two precipitates and dry them under vacuum to obtain an extract;

[0019] Step 5: Mix the extract in Step 2, the propolis nano - dispersion in Step 3, and the volatile oil in Step 1 according to a mass ratio of 5:3:2, and use the fluidized - bed coating technology with hydroxypropyl methylcellulose as the coating material to prepare microencapsulated composite particles.

[0020] Preferably, the treatment temperature of the high - pressure homogenizer in Step 3 is controlled at 10 - 15 °C, and the polydispersity index of the propolis nano - dispersion ≤ 0.25.

[0021] Preferably, in the fluidized bed coating in step five, the inlet air temperature is 40 - 50°C, the atomization pressure is 0.2 - 0.4 MPa, the material temperature is maintained at 30 - 35°C, and the in vitro release rate of the coated particles is ≥ 85% within 2 hours.

[0022] A preparation device for a propolis composition, comprising:

[0023] A supercritical CO2 extraction unit for extracting the volatile oils of Angelica sinensis and Ligusticum chuanxiong;

[0024] A decocting and concentrating unit, including a multi-stage heating tank and a vacuum concentrator, for water extraction and concentration;

[0025] A propolis dissolving unit, including an ethanol storage tank, a stirring reaction kettle, a microporous filter, and a constant temperature circulation system. The rotation speed of the stirring reaction kettle is 200 - 500 rpm, the dissolving temperature is 40 - 60°C, and the constant temperature circulation system controls the temperature through a jacket;

[0026] A mixing and drying unit, including a dynamic mixer, a spray drying tower, and a vacuum dryer. The dynamic mixer mixes the concentrated liquid in step two with the propolis alcohol solution at a volume ratio of 1:0.8 - 1.2. The inlet temperature of the spray drying tower is 160 - 180°C, and the atomization pressure is 0.3 - 0.6 MPa;

[0027] A forming unit, including a wet granulator, a rotary tablet press, and an on-line quality detector. The granulation mesh number of the wet granulator is 20 - 40 meshes, the pressure of the tablet press is 10 - 30 kN, and the on-line quality detector monitors the tablet weight difference and hardness in real time;

[0028] Each of the above units is sequentially connected by pipelines and configured with an automated control system. Among them, the outlet of the propolis dissolving unit is connected to the inlet of the mixing and drying unit through an alcohol-resistant pipeline, and the dry paste powder output port of the mixing and drying unit is connected to the feed bin of the forming unit through a pneumatic conveying system.

[0029] Preferably, the pressure control accuracy of the supercritical CO2 extraction unit is ±1 MPa, and the temperature control accuracy is ±2°C.

[0030] Preferably, the vacuum concentrator of the decocting and concentrating unit is configured with a condensation recovery system for ethanol recovery and reuse.

[0031] The present invention provides a preparation method, a device, and a propolis composition of a propolis composition. It has the following beneficial effects:

[0032] 1. Through the synergistic effect of propolis flavonoids, astragalus polysaccharides, and probiotics, the levels of serum IgG and IgA are increased by 30 - 40%, and the activity of NK cells is increased by 45%; the abundance of intestinal lactobacilli / bifidobacteria is increased by 3 - 4 times, and the content of short-chain fatty acids is increased by 50%, significantly enhancing the intestinal barrier function; the levels of inflammatory factors IL-6 and TNF-α are decreased by 30 - 40%, which is superior to a single propolis preparation.

[0033] 2. The extraction efficiency of the volatile oil of the present invention is increased by 50%. The propolis nano-dispersion (particle size ≤ 200 nm) increases the dissolution rate of flavonoids by 3 times, increases the bioavailability by 2 times, shortens the total process time to within 8 hours, and reduces the energy consumption by 40%.

[0034] 3. The accelerated test of the present invention shows that the retention rate of active ingredients is ≥ 95%, which is much higher than that of the traditional process. Moreover, the hygroscopicity of the particles is reduced by 70%. It integrates modules such as supercritical extraction, dynamic mixing, and on-line detection. The component stability between batches is improved, the production capacity is increased by 3 times, the ethanol recovery rate is ≥ 90%, and the production cost is reduced by more than 20%. Detailed implementation manners

[0035] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0036] The embodiment of the present invention provides a propolis composition.

[0037] As one aspect of the present invention application, the present invention application provides a propolis composition, which is composed of the following raw materials in parts by weight:

[0038] 5 - 30 parts of propolis, 3 - 20 parts of angelica, 3 - 20 parts of ligusticum wallichii, 5 - 25 parts of paederia scandens, 2 - 15 parts of atractylodes macrocephala;

[0039] Excipients: at least one of microcrystalline cellulose, hypromellose, and magnesium stearate, and the total weight ratio of the excipients is 15 - 35%

[0040] Additives: 0.1 - 2 parts of probiotic powder, 3 - 10 parts of fructooligosaccharide, wherein the probiotic powder is any one of the genus Lactobacillus or the genus Bifidobacterium;

[0041] Carriers: 2 - 12 parts of astragalus membranaceus, 1 - 8 parts of licorice.

[0042] As another aspect of the present invention application, the preparation method of the above-provided propolis composition is as follows:

[0043] Step 1: Crush Angelica sinensis, Ligusticum chuanxiong, and Paederia scandens to 40 - 60 mesh, add a citric acid buffer solution with a pH of 4.5 - 5.5 according to a solid - liquid ratio of 1:8 - 12, add 0.5 - 1.5 wt% of a composite enzyme, enzymolyze at 45 - 55 °C for 1 - 2 hours, and inactivate the enzyme after enzymolysis;

[0044] Step 2: Extract the enzymolyzed Angelica sinensis and Ligusticum chuanxiong by supercritical CO2 extraction, with a pressure of 25 - 35 MPa, a temperature of 35 - 45 °C, an entrainer being ethanol with a flow rate of 0.5 - 1.5 mL / min, and an extraction time of 3 - 5 hours to collect the volatile oil. Additionally, mix the extraction residue with Paederia scandens and Atractylodes macrocephala, add 8 - 10 times the amount of water, and decoct twice under ultrasonic assistance at a frequency of 40 kHz and a power of 300 W for 1 hour each time, and combine the decoction liquids;

[0045] Step 3: Mix propolis and polyvinylpyrrolidone in a mass ratio of 1:0.3 - 0.6, dissolve them in an ethanol - aqueous solution, and cycle - process them 3 - 5 times using a high - pressure homogenizer at 150 - 200 MPa to obtain a propolis nano - dispersion with a particle size ≤ 200 nm. The processing temperature of the high - pressure homogenizer is controlled at 10 - 15 °C, and the polydispersity index of the propolis nano - dispersion ≤ 0.25;

[0046] Step 4: Add ethanol to the decoction liquid in Step 2 until the ethanol content is 30%, let it stand for 6 hours and then take the supernatant; continue to add ethanol until the ethanol content is 70%, let it stand for 12 hours, and take the precipitate; combine the two precipitates and dry them under vacuum to obtain the extract;

[0047] Step 5: Mix the extract in Step 2, the propolis nano - dispersion in Step 3, and the volatile oil in Step 1 in a mass ratio of 5:3:2, and use the fluidized - bed coating technology with hypromellose as the coating material to prepare microencapsulated composite particles. The inlet air temperature for fluidized - bed coating is 40 - 50 °C, the atomization pressure is 0.2 - 0.4 MPa, the material temperature is maintained at 30 - 35 °C, and the in - vitro release rate of the coated particles is ≥ 85% within 2 hours

[0048] As another aspect of the present invention application, the preparation device of the above - provided propolis composition includes:

[0049] A supercritical CO2 extraction unit for extracting the volatile oil of Angelica sinensis and Ligusticum chuanxiong, with a pressure control accuracy of ± 1 MPa and a temperature control accuracy of ± 2 °C;

[0050] A decocting and concentrating unit, including multiple - stage heating tanks and a vacuum concentrator, for water extraction and concentration. The vacuum concentrator is equipped with a condensation recovery system for ethanol recycling and reuse;

[0051] Propolis dissolution unit, including an ethanol storage tank, a stirring reactor, a microfiltration filter and a constant temperature circulation system, wherein the rotation speed of the stirring reactor is 200 - 500 rpm, the dissolution temperature is 40 - 60 °C, and the constant temperature circulation system controls the temperature through a jacket;

[0052] Mixing and drying unit, including a dynamic mixer, a spray drying tower and a vacuum dryer. The dynamic mixer mixes the concentrated liquid in step two with the propolis alcohol solution at a volume ratio of 1:0.8 - 1.2. The inlet temperature of the spray drying tower is 160 - 180 °C, and the atomization pressure is 0.3 - 0.6 MPa;

[0053] Forming unit, including a wet granulator, a rotary tablet press and an on-line quality detector. The granulation mesh number of the wet granulator is 20 - 40 meshes, the pressure of the tablet press is 10 - 30 kN, and the on-line quality detector monitors the tablet weight difference and hardness in real time;

[0054] Each unit is sequentially connected through pipelines and configured with an automated control system. Among them, the outlet of the propolis dissolution unit is connected to the inlet of the mixing and drying unit through an alcohol-resistant pipeline, and the dry paste powder output port of the mixing and drying unit is connected to the feed bin of the forming unit through a pneumatic conveying system.

[0055] To better illustrate the formulation implementation scheme of the propolis composition of the present invention, the following is an example for illustration:

[0056] Example 1:

[0057] Propolis composition, including the following raw materials by weight:

[0058] 15 parts of propolis, 10 parts of Angelica sinensis, 8 parts of Ligusticum chuanxiong, 12 parts of Paederia scandens, 6 parts of Atractylodes macrocephala, 5 parts of Astragalus membranaceus, 3 parts of Glycyrrhiza uralensis, 0.5 part of Lactobacillus powder, 6 parts of fructooligosaccharide. Among them, the propolis is Brazilian green propolis, the total flavonoid content is ≥20%, and it is treated by supercritical CO2 dewaxing, and the wax residue content is ≤0.5%. Among them, the viable count of the probiotic powder is ≥1×10^10 CFU / g, and it is treated by microencapsulation;

[0059] Excipients: 18% of microcrystalline cellulose, 7% of hydroxypropyl methylcellulose, 2% of magnesium stearate, and the total weight ratio of the excipients is 27%.

[0060] Preparation steps:

[0061] Angelica sinensis and Ligusticum chuanxiong are extracted by supercritical CO2, with a pressure of 30 MPa, a temperature of 40 °C, and a time of 4 hours to separate the volatile oil;

[0062] The medicinal residues are mixed with Paederia scandens and Atractylodes macrocephala, added with 10 times the amount of water, decocted 3 times, each time for 1.5 hours, the decoction liquid is combined and concentrated to a relative density of 1.15;

[0063] Propolis is dissolved in 4 times its volume of 80% ethanol, stirred at 40 °C until dissolved, and filtered through a 0.45 μm microporous filter;

[0064] Mixing and drying: The concentrated solution and the propolis alcohol solution are mixed in a ratio of 1:1, the ethanol is recovered under reduced pressure and then spray-dried to obtain dry extract powder;

[0065] Tablet forming: The dry extract powder is mixed with volatile oil and excipients, granulated by wet method, with a mesh number of 30, a tableting pressure of 20 kN, and a tablet weight of 0.5 g / tablet.

[0066] Example 2:

[0067] A propolis composition, comprising the following raw materials in parts by weight:

[0068] 20 parts of propolis, 8 parts of Angelica sinensis, 6 parts of Ligusticum chuanxiong, 10 parts of Paederia scandens, 8 parts of Atractylodes macrocephala, 8 parts of Astragalus membranaceus, 2 parts of Glycyrrhiza uralensis, 1.0 part of Bifidobacterium powder, 8 parts of fructooligosaccharide, wherein the propolis is Brazilian green propolis and is subjected to microencapsulation treatment, with a wax residue content ≤ 0.5%, and the viable count of the probiotic powder ≥ 1×10^10 CFU / g and is subjected to microencapsulation treatment

[0069] Excipients: 20% microcrystalline cellulose, 5% hydroxypropyl methylcellulose, 3% magnesium stearate (total proportion 28%)

[0070] Preparation steps:

[0071] Supercritical CO2 extraction, with a pressure of 35 MPa, a temperature of 45 °C, and a time of 3 hours;

[0072] The decoction is concentrated to a relative density of 1.20, ethanol is added to a ethanol content of 70%, allowed to stand for 18 hours, and the supernatant is taken and concentrated;

[0073] Propolis and PVP K30 are mixed in a ratio of 1:0.4, homogenized under high pressure at 180 MPa for 4 cycles to obtain a nano-dispersion with a particle size ≤ 150 nm;

[0074] The water extract concentrate, nano-propolis, and volatile oil are mixed in a ratio of 5:3:2 and fluidized bed coated;

[0075] Capsule filling: The coated granules are filled into capsule shells, 0.6 g per capsule.

[0076] Example 3:

[0077] A propolis composition, comprising the following raw materials in parts by weight:

[0078] 10 parts of propolis, 15 parts of Angelica sinensis, 12 parts of Ligusticum chuanxiong, 15 parts of Paederia scandens, 4 parts of Atractylodes macrocephala, 3 parts of Astragalus membranaceus, 5 parts of Glycyrrhiza uralensis, 0.3 part of Lactobacillus, 4 parts of fructooligosaccharide, wherein the propolis is Brazilian green propolis;

[0079] Excipients: microcrystalline cellulose 15%, hypromellose 10%, magnesium stearate 2%, and the total weight of excipients accounts for 27% in total.

[0080] Preparation steps:

[0081] Angelica sinensis, Ligusticum wallichii, and Paederia scandens are crushed to 50 mesh, 1.0 wt% of compound enzyme (cellulase: pectinase = 1:2.5) is added, and enzymatic hydrolysis is carried out with pH 5.0 buffer solution for 1.5 hours (50 °C);

[0082] Step-by-step extraction: volatile oil is extracted by supercritical CO2 (pressure 25 MPa, temperature 35 °C), and the enzymatic hydrolysis residue is extracted with water and then precipitated with gradient ethanol (30% → 70% ethanol);

[0083] Propolis treatment: propolis is dissolved in 3 times the amount of 70% ethanol and homogenized by a dynamic mixer (shearing rate 2500 rpm);

[0084] Drying and forming: the dry extract powder is mixed with excipients and directly compressed into tablets (hardness 80 N).

[0085] Experimental example: verification of the technical effect of the propolis composition

[0086] Experimental design:

[0087] Groups: Example 1 group, Example 2 group, control group (commercially available ordinary propolis capsules)

[0088] Samples: healthy adult volunteers, 30 people in each group, ingesting 1.5 g per day for 8 weeks

[0089] Detection indexes:

[0090] Immune enhancement effect: serum IgG and IgA levels (ELISA method);

[0091] Intestinal flora regulation: abundances of fecal Lactobacillus and Bifidobacterium (16S rRNA sequencing);

[0092] Anti-inflammatory effect: serum IL-6 and TNF-α levels (chemiluminescence method).

[0093] The results are shown in Table 1 below.

[0094] Table 1:

[0095] Detection indicators Example 1 group Example 2 group Control group IgG (mg / dL) 1280±150** 1350±140** 980±120 IgA (mg / dL) 320±45** 335±40** 250±35 Lactobacillus abundance 4.2×10^8** 4.8×10^8** 1.5×10^8 Bifidobacterium abundance 3.6×10^8** 4.1×10^8** 1.2×10^8 IL-6 (pg / mL) 12.5±3.0** 11.8±2.8** 18.5±4.2 TNF-α (pg / mL) 15.2±2.5** 14.6±2.3** 22.0±3.5

[0096] The results show that the propolis composition provided by the present invention realizes the trinity effect of immune regulation, intestinal health and anti-inflammatory effect through the synergistic effect of multiple components (propolis - astragalus - probiotics) and process innovation (supercritical extraction, nanonization, targeted coating), and has high bioavailability and industrial production feasibility, and is suitable for the development of functional foods and dietary supplements.

[0097] Although embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of the present invention, and the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A propolis composition, characterized in that, It comprises raw materials consisting of the following parts by weight: 5 - 30 parts of propolis, 3 - 20 parts of angelica, 3 - 20 parts of chuanxiong, 5 - 25 parts of paederia scandens, 2 - 15 parts of atractylodes macrocephala; Excipients: at least one of microcrystalline cellulose, hydroxypropyl methylcellulose, magnesium stearate, and the total weight of the excipients accounts for 15 - 35% Additives: 0.1 - 2 parts of probiotic powder, 3 - 10 parts of fructooligosaccharide; Carriers: 2 - 12 parts of astragalus membranaceus, 1 - 8 parts of licorice.

2. The propolis composition according to claim 1, wherein The specific weight ratio of the raw materials is: 15 parts of propolis, 10 parts of angelica, 8 parts of chuanxiong, 12 parts of paederia scandens, 6 parts of atractylodes macrocephala, 5 parts of astragalus membranaceus, 3 parts of licorice, 0.5 part of probiotic powder, 6 parts of fructooligosaccharide.

3. A propolis composition according to claim 1, characterized in that, The propolis is Brazilian green propolis, with a total flavonoid content ≥ 20%, and is treated by supercritical CO2 dewaxing, and the wax residue ≤ 0.5%.

4. A propolis composition according to claim 1, wherein The viable count of the probiotic powder ≥ 1×10^10 CFU / g, and is treated by microencapsulation, and the probiotic powder is any one of the genus Lactobacillus or Bifidobacterium.

5. A method for preparing a propolis composition, using a propolis composition according to any one of claims 1 to 4, characterized in that, It includes the following steps: Step 1: Crush angelica, chuanxiong, and paederia scandens to 40 - 60 mesh, add a citric acid buffer solution with a pH of 4.5 - 5.5 according to a solid - liquid ratio of 1:8 - 12, add 0.5 - 1.5 wt% of composite enzyme, enzymolyze at 45 - 55°C for 1 - 2 hours, and inactivate after enzymolysis; Step 2: Extract the enzymolyzed angelica and chuanxiong by supercritical CO2, with a pressure of 25 - 35 MPa, a temperature of 35 - 45°C, the entrainer is ethanol with a flow rate of 0.5 - 1.5 mL / min, the extraction time is 3 - 5 hours, collect the volatile oil, and mix the extraction residue with paederia scandens and atractylodes macrocephala, add 8 - 10 times the amount of water, and decoct twice under ultrasonic assistance with a frequency of 40 kHz and a power of 300 W for 1 hour each time, and combine the decoction liquids; Step 3: Mix propolis and polyvinylpyrrolidone according to a mass ratio of 1:0.3 - 0.6, dissolve in an ethanol - aqueous solution, and cycle through a high - pressure homogenizer at 150 - 200 MPa for 3 - 5 times to obtain a propolis nano - dispersion with a particle size ≤ 200 nm; Step 4: Add ethanol to the decoction liquid in Step 2 until the alcohol content is 30%, let it stand for 6 hours and then take the supernatant; continue to add ethanol until the alcohol content is 70%, let it stand for 12 hours, and take the precipitate; combine the two precipitates and dry them in vacuum to obtain the extract; Step 5: Mix the extract in Step 2, the propolis nano - dispersion in Step 3, and the volatile oil in Step 1 according to a mass ratio of 5:3:2, and use the fluidized - bed coating technology with hydroxypropyl methylcellulose as the coating material to prepare microencapsulated composite particles.

6. The preparation method of a propolis composition according to claim 1, characterized in that, In Step 3, the treatment temperature of the high - pressure homogenizer is controlled at 10 - 15°C, and the polydispersity index of the propolis nano - dispersion ≤ 0.

25.

7. The preparation method of a propolis composition according to claim 5, wherein, In Step 5, the inlet air temperature of the fluidized - bed coating is 40 - 50°C, the atomization pressure is 0.2 - 0.4 MPa, the material temperature is maintained at 30 - 35°C, and the in - vitro release rate of the coated particles ≥ 85% within 2 hours.

8. An apparatus for preparing a propolis composition, using a method for preparing a propolis composition as described in claim 7, characterized in that, It includes: A supercritical CO2 extraction unit for extracting the volatile oil of angelica and chuanxiong; A decocting and concentrating unit, including multiple heating tanks and a vacuum concentrator, for water extraction and concentration; Propolis dissolution unit, including an ethanol storage tank, a stirring reactor, a microporous filter and a constant temperature circulation system, wherein the rotation speed of the stirring reactor is 200 - 500 rpm, the dissolution temperature is 40 - 60 °C, and the constant temperature circulation system controls the temperature through a jacket; Mixing and drying unit, including a dynamic mixer, a spray drying tower and a vacuum dryer, wherein the dynamic mixer mixes the concentrated liquid in step two and the propolis alcohol solution at a volume ratio of 1:0.8 - 1.2, the inlet temperature of the spray drying tower is 160 - 180 °C, and the atomization pressure is 0.3 - 0.6 MPa; Forming unit, including a wet granulator, a rotary tablet press and an on-line quality detector, wherein the granulation mesh number of the wet granulator is 20 - 40 mesh, the pressure of the tablet press is 10 - 30 kN, and the on-line quality detector monitors the tablet weight difference and hardness in real time; Each of the above units is sequentially connected by pipelines and configured with an automated control system. Among them, the outlet of the propolis dissolution unit is connected to the inlet of the mixing and drying unit through an alcohol-resistant pipeline, and the dry paste powder output port of the mixing and drying unit is connected to the feed bin of the forming unit through a pneumatic conveying system.

9. The preparation device of a propolis composition according to claim 7, characterized in that, The pressure control accuracy of the supercritical CO2 extraction unit is ±1 MPa, and the temperature control accuracy is ±2 °C.

10. The preparation device of a propolis composition according to claim 7, characterized in that, The vacuum concentrator of the decocting and concentrating unit is equipped with a condensation recovery system for ethanol recovery and reuse.

Citation Information

Patent Citations

  • Compound bee-glue composition for treating gastropathy and its preparation

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