CN111000881B - Propolis soft capsule rich in flavone and belonging to genus Brazilian breynia and preparation method thereof - Google Patents

Propolis soft capsule rich in flavone and belonging to genus Brazilian breynia and preparation method thereof Download PDF

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CN111000881B
CN111000881B CN201911373902.9A CN201911373902A CN111000881B CN 111000881 B CN111000881 B CN 111000881B CN 201911373902 A CN201911373902 A CN 201911373902A CN 111000881 B CN111000881 B CN 111000881B
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propolis
brazilian
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ethanol solution
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CN111000881A (en
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刘嘉
周荣
赵继敏
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Fengnaibao Benpu Nanjing Health Care Food Co ltd
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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)
    • A61K36/25—Araliaceae (Ginseng family), e.g. ivy, aralia, schefflera or tetrapanax
    • A61K36/258—Panax (ginseng)
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K35/00—Medicinal preparations containing materials or reaction products thereof with undetermined constitution
    • A61K35/56—Materials from animals other than mammals
    • A61K35/63—Arthropods
    • A61K35/64—Insects, e.g. bees, wasps or fleas
    • A61K35/644—Beeswax; Propolis; Royal jelly; Honey
    • 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
    • A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/4841—Filling excipients; Inactive ingredients
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    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30—Extraction of the material
    • A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/55—Liquid-liquid separation; Phase separation

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Abstract

The invention discloses a flavonoid-rich Brazilian breynia type propolis soft capsule, which comprises a capsule shell and capsule contents, wherein the capsule contents comprise the following components in parts by weight: 10-15 parts of Brazilian breynia propolis extract, 9-13 parts of compound flavone extract and 1-5 parts of beeswax; the capsule shell comprises the following components in parts by weight: 25-30 parts of gelatin, 5-10 parts of glycerol and 25-35 parts of purified water. The preparation method comprises the following steps: preparing a Brazilian alcohol chrysanthemum genus propolis extract by an ethanol extraction method; by using supercritical CO2Extracting to obtain compound flavone extract; mixing the propolis extract, the compound flavone extract and the beeswax according to the formula proportion, heating and stirring uniformly; degassing and defoaming by twice vacuum colloid mills, mixing and stirring gelatin and glycerol in proportion for 1.5-2h, mixing with purified water, and filtering to obtain gelatin solution with certain viscosity and water content; filling the qualified semi-finished propolis mixed solution of Chrysanthemum morifolium L to obtain soft capsule.

Description

Propolis soft capsule rich in flavone and belonging to genus Brazilian breynia and preparation method thereof
Technical Field
The invention relates to a Brazilian breynia type propolis soft capsule rich in flavone and a preparation method thereof, belonging to the technical field of propolis extraction.
Background
Propolis is a colloidal solid prepared by collecting plant resin secretion from western bee, mixing with secretion from own body such as jawbone and cerifera, and processing. The propolis has complex chemical components, is a complex system with multiple components and multiple target points, has various biological activities of bacteriostasis, antioxidation, anti-inflammation, immunoregulation, anti-tumor and the like, and is widely applied to the fields of medicine, health care, daily chemicals and the like.
The glue source plant is an important factor influencing the chemical components and the biological activity of the propolis. In southeast and midwest regions of brazil, brazil canthus type derived from cantonese plant is subject to additional use in the world propolis market due to its unique chemical components and strong health care efficacy, and cantonese type propolis contains phenolic acids, terpenes, and also contains special substance such as atopirin C, and has special aromatic odor and multiple biological activities. Since this propolis is rich in bioflavonoids and has a green-brown strip-like appearance, it is called Brazilian chamomilla type, and its apiolin C is the most abundant of propolis.
Because of the complex components in the Brazilian holly chrysanthemum type, the propolis in the Brazilian holly chrysanthemum type needs to be added before the useThe effective components in the extract are extracted, and phenolic acid, flavonoid and atopizin C in the Brazilian alcohol chrysanthemum type are mainly extracted, wherein the extraction mode aiming at the Brazilian alcohol chrysanthemum type mainly comprises the following steps: 1. ethanol and petroleum ether two-phase solvent extraction method; 2. sodium hydroxide solvent extraction; 3. ethanol solution dipping method; 4. supercritical CO2And (4) an extraction method. The ethanol solution dipping method has the best extraction effect in the actual extraction process, but the prior ethanol solution dipping method has the following defects in the extraction process of the Brazilian callistemon type:
in the existing extraction process aiming at the Brazilian ethanol, phenolic acid, flavonoid, alistipine C and other components in the Brazilian ethanol are uniformly extracted, so that the maximum utilization of the Brazilian ethanol cannot be realized, and a part of phenolic acid, flavonoid, alistipine C and other components are not effectively extracted; and part of the functional components in the ethanol-extracted propolis residues are not obtained yet.
Propolis is usually prepared into a capsule product after being extracted, and the capsule product can improve blood circulation and reduce blood fat after being taken for a long time; the flavonoid component in propolis also has antibacterial and antioxidant effects. In order to obtain better antibacterial and antioxidant effects, the higher the content of flavonoids in the propolis capsule, the better the content, and the limited content of flavonoids in the existing propolis capsule.
As is well known, ginseng has a very good medicinal value; recent research shows that ginseng leaves and ginseng roots have similar pharmacological effects. The main components of the ginseng leaf are ginsenoside components and ginseng flavonoid components, and have the effects of improving the human body immunity, promoting substance metabolism, resisting aging and the like. In the prior art, the ginseng leaf extract and the propolis capsule are organically combined.
Disclosure of Invention
The purpose is as follows: in order to overcome the defects in the prior art, the invention provides a Brazilian ethanol chrysanthemum type propolis soft capsule rich in flavone and a preparation method thereof.
The technical scheme is as follows: in order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the propolis soft capsule rich in flavone in Brazilian neriifolia belongs to the genus of propolis comprises a capsule shell and capsule contents, wherein the capsule contents comprise the following components in parts by weight: 10-15 parts of Brazilian breynia propolis extract, 9-13 parts of compound flavone extract and 1-5 parts of beeswax;
the capsule shell comprises the following components in parts by weight: 25-30 parts of gelatin, 5-10 parts of glycerol and 25-35 parts of purified water.
A method for preparing propolis soft capsule rich in flavone in Brazilian Chrysanthemum comprises the following steps:
(1) preparing Brazilian brevifolius type propolis extract D by ethanol extraction;
(2) by using supercritical CO2Extracting to obtain compound flavone extract F;
(3) mixing the Brazilian callistemon type propolis extract D, the compound flavone extract F and the beeswax according to a formula ratio, heating, and uniformly stirring to ensure that the components are as follows in parts by weight: 10-15 parts of Brazilian brevifolius propolis extract, 10-13 parts of compound flavone extract F9, and 1-5 parts of beeswax;
(4) degassing and defoaming the mixed solution by twice vacuum colloid mills to obtain qualified alcohol chrysanthemum type propolis semi-finished product mixed solution, and keeping the temperature at 45-50 ℃ for later use;
(5) mixing gelatin and glycerol at a certain ratio, stirring for 1.5-2h, mixing with purified water, filtering to obtain gelatin solution with certain viscosity and water content, filling the qualified semi-finished product mixture of JIUSHENGJU type propolis obtained in step (4) into soft capsule, pressing, shaping, washing, drying, inspecting, packaging, inspecting, and warehousing.
Further, the preparation method of the Brazilian nerium type propolis extract D is as follows:
1.1) taking a proper amount of Brazilian wine Shen type propolis raw material, and freezing and storing for 16-24 hours at the temperature of-4 to-10 ℃;
1.2) crushing the propolis raw material frozen in the step 1.1) by using a universal crusher for 10-15 minutes, and adding a crushing medium in the crushing process; screening by using a vibrating screen after crushing, wherein the mesh number of the vibrating screen is 40-60 meshes;
1.3) dividing the propolis raw materials screened in the step 1.2) into three equal parts, and marking the three equal parts as a propolis raw material A, a propolis raw material B and a propolis raw material C;
1.4) extracting three equal parts of the propolis raw materials A, B, C in the step 1.3) in three ethanol solutions with different concentrations respectively, wherein the concentration of the ethanol solution is 75-95%, and the specific extraction process is as follows:
1.4.1) preparing the propolis raw material A: ethanol solution E11: adding propolis raw material A into ethanol solution E at a ratio of 6W/V1Extracting at 25 deg.C for 24 hr while stirring and ultrasonic extracting, and collecting propolis extractive residue A0Pumping the supernatant after the leaching and leaching into a settling tank at the temperature of-6-0 ℃, cooling and settling for 36 hours, filtering the settling liquid by a filter screen with a plate frame of 400 meshes, and collecting the filtered filtrate LA；
1.4.2) according to the propolis raw material B: ethanol solution E21: 6W/V, adding propolis raw material B into ethanol solution E2Extracting at 25 deg.C for 24 hr while stirring and ultrasonic extracting, and collecting propolis residue B0Pumping the supernatant after the leaching and leaching into a settling tank at the temperature of-6-0 ℃, cooling and settling for 36 hours, filtering the settling liquid by a filter screen with a plate frame of 400 meshes, and collecting the filtered filtrate LB；
1.4.3) according to the propolis raw material C: ethanol solution E31: 6W/V, adding propolis material C into ethanol solution E3Extracting at 25 deg.C for 24 hr while stirring and ultrasonic extracting, and collecting propolis residue C0Pumping the supernatant after the leaching and leaching into a settling tank at the temperature of-6-0 ℃, cooling and settling for 36 hours, filtering the settling liquid by a filter screen with a plate frame of 400 meshes, and collecting the filtered filtrate LC；
1.5) the filtrate L obtained in step 1.4)A、LB、LCMixing, and concentrating in a vacuum evaporator to obtain propolis extract D.
Further, the preparation method of the compound flavone extract F comprises the following steps:
2.1) removing impurities from the ginseng leaves, drying, and crushing the dried ginseng leaves; extracting the propolis extraction residue A in the step 1.4)0、B0And C0Mixing, drying, crushing, mixing with crushed ginseng leaves in equal mass, and sieving with a 18-35 mesh sieve to obtain composite raw material powder;
2.2) adding CO into the composite raw material powder obtained in the step 2.1)2Adding an entrainer absolute ethyl alcohol into a supercritical extractor, performing supercritical extraction at an extraction pressure of 25-35 MPa, a fluid flow rate of 0.5-1 mL/min and an extraction temperature of 40-55 ℃ for 1-3h, and collecting an extract after the extraction is finished to obtain a compound flavone crude extract solution;
2.3) carrying out suction filtration and concentration on the crude extract solution of the compound flavone, diluting the concentrated extract solution with 15-20% ethanol solution, cooling the diluted extract solution for 8-11 hours at the temperature of 3-5 ℃, and carrying out suction filtration again to prepare upper column solution;
2.4) eluting the column loading liquid AB-8 resin column in the step 2.3) by pure water, eluting the resin column by 20-60% ethanol solution, and collecting eluent; concentrating the eluate by rotary evaporation, and vacuum drying to obtain compound flavone extract F.
Further, the crushing medium is rice hulls, rice bran or wheat bran.
Further, ethanol solution E in the step 1.4)1Is 75%, ethanol solution E2Of 85%, ethanol solution E3The concentration of (3) is 95%.
Further, in the step 1.4.1), the step 1.4.2) and the step 1.4.3), the regular stirring is performed once every 3 hours for 30min, and the stirring speed of the regular stirring is 150-200 rpm.
Further, in the step 1.4.1), the step 1.4.2) and the step 1.4.3), the ultrasonic wave is intensified to be ultrasonic once every 4 hours, and the ultrasonic power is 1000W.
Further, in the step 1.5), the mixed filtrate is placed into a decompression evaporator, and is heated by adopting a water bath, wherein the evaporation temperature is 35-50 ℃, and the vacuum degree is 0.1 MPa.
Has the advantages that: the invention provides a Brazilian ethanol chrysanthemum type propolis soft capsule rich in flavone and a preparation method thereof, wherein filtrate obtained after extraction in 75% ethanol solution, 85% ethanol solution and 95% ethanol solution is mixed and concentrated, and the contents of phenolic acid, flavonoid and atopizin C in the obtained propolis extract can reach higher levels, so that the application of the Brazilian ethanol chrysanthemum type is optimized; mixing the rest propolis extracted with ethanol with folium Ginseng, and supercritical CO extraction2The extraction method is used for extracting the flavonoid compounds in the mixture, so that the effective components of the propolis are fully extracted, and the ginseng leaves are rich in the flavonoid compounds, so that the content of the flavonoid components is further increased; simultaneous supercritical CO2The extraction method has the advantages of low energy consumption, high flavone yield and low potential safety hazard.
Detailed Description
The present invention will be further described with reference to the following examples.
The propolis soft capsule rich in flavone in Brazilian neriifolia belongs to the genus of propolis comprises a capsule shell and capsule contents, wherein the capsule contents comprise the following components in parts by weight: 10-15 parts of Brazilian breynia propolis extract, 9-13 parts of compound flavone extract and 1-5 parts of beeswax; the capsule shell comprises the following components in parts by weight: 25-30 parts of gelatin, 5-10 parts of glycerol and 25-35 parts of purified water.
Preferably, the propolis soft capsule rich in flavone in Brazilian neriifolia genus comprises a capsule shell and a capsule content, wherein the capsule content comprises the following components in parts by weight: 12 parts of Brazilian callistemon herb type propolis extract, 11 parts of compound flavone extract and 3 parts of beeswax; the capsule shell comprises the following components in parts by weight: 25 parts of gelatin, 8 parts of glycerol and 30 parts of purified water.
A method for preparing propolis soft capsule rich in flavone in Brazilian Chrysanthemum comprises the following steps:
(1) the ethanol extraction method is adopted to prepare the Brazilian alcohol chrysanthemum genus propolis extract D, and the specific steps are as follows:
1.1) taking a proper amount of Brazilian spirit type propolis raw material, and freezing and storing for 16-24 hours at the temperature of-4 to-10 ℃.
1.2) crushing the propolis raw material frozen in the step 1.1) by using a universal crusher for 10-15 minutes, and adding a crushing medium in the crushing process; screening by using a vibrating screen after crushing, wherein the mesh number of the vibrating screen is 40-60 meshes;
the crushing medium is rice husk, rice bran or wheat bran, and can avoid the mutual adhesion or adhesion of propolis plastification and plasticizing on a universal crusher caused by temperature rise in the crushing process.
1.3) dividing the propolis raw materials screened in the step 1.2) into three equal parts, and marking the three equal parts as a propolis raw material A, a propolis raw material B and a propolis raw material C.
1.4) dividing the propolis raw material A in the step 1.3) into two equal parts of A1 and A2, dividing the propolis raw material B into two equal parts of B1 and B2, and dividing the propolis raw material C into two equal parts of C1 and C2; dissolving A1 and A2 in 75% ethanol solution E1Extracting with ethanol solution E of 85% ethanol solution B1 and B22Extracting with C1 and C2 in 95% ethanol solution E3Extracting;
the specific extraction process is as follows:
1.4.1) preparing the propolis raw materials A1 and A2: ethanol solution E11: 6W/V, A1 and A2 each 10g in mass, 60ml of ethanol solution E1Leaching for 24 hours at 25 ℃, carrying out ultrasonic enhanced extraction by timing stirring and ultrasonic waves in the leaching process, wherein the ultrasonic power is 1000W, the timing stirring is carried out once every 3 hours, the stirring is carried out once for 30min, and the timing stirring speed is 150-200 rpm; collecting propolis extraction residue A after leaching10、A20Pumping the supernatant after the leaching and leaching into a settling tank at the temperature of-6-0 ℃, cooling and settling for 36 hours, and filtering the settling liquid through a plate frame, wherein the mesh number of the plate frame is 400 meshes; filtrate L of A1 after filtrationA1Putting into a reduced pressure evaporator, heating in water bath at an evaporation temperature of 35-50 deg.C and a vacuum degree of above 0.1MPa, and concentrating to obtain propolis extract A1'; collecting filtrate L of A2 after filtrationA2；
1.4.2) mixing the propolis raw materials B1 and B2: ethanol solution E21: the weight of B1 and B2 is 10g, and 60ml of ethanol solution E is added respectively2In the leaching at 25 ℃ of 24h, performing timed stirring and ultrasonic enhanced extraction in the leaching process, performing ultrasonic treatment once every 4 hours, wherein the ultrasonic power is 1000W, the timed stirring is performed once every 3 hours, the stirring is performed for 30min once, and the timed stirring speed is 150-200 rpm; collecting propolis extraction residue B after leaching10、B20Pumping the supernatant after the leaching and leaching into a settling tank at the temperature of-6-0 ℃, cooling and settling for 36 hours, and filtering the settling liquid through a plate frame, wherein the mesh number of the plate frame is 400 meshes; filtrate L of filtered B1B1Putting into a reduced pressure evaporator, heating in water bath at an evaporation temperature of 35-50 deg.C and a vacuum degree of above 0.1MPa, and concentrating to obtain propolis extract B1'; collecting filtrate L of B2 after filtrationB2；
1.4.3) according to the propolis raw material C: ethanol solution E31: the weight of C1 and C2 is 10g, and 60ml of ethanol solution E is added respectively3Leaching for 24 hours at 25 ℃, carrying out ultrasonic enhanced extraction by timing stirring and ultrasonic waves in the leaching process, wherein the ultrasonic power is 1000W, the timing stirring is carried out once every 3 hours, the stirring is carried out once for 30min, and the timing stirring speed is 150-200 rpm; collecting propolis extraction residue C after leaching10、C20Pumping the supernatant after the leaching and leaching into a settling tank at the temperature of-6-0 ℃, cooling and settling for 36 hours, and filtering the settling liquid through a plate frame, wherein the mesh number of the plate frame is 400 meshes; filtrate L of filtered C1C1Putting into a reduced pressure evaporator, heating in water bath at an evaporation temperature of 35-50 deg.C and a vacuum degree of above 0.1MPa, and concentrating to obtain propolis extract C1'; collecting filtrate L of C2 after filtrationC2。
1.5) the filtrate L obtained in step 1.4)A2、LB2、LC2Mixing, and concentrating in a vacuum evaporator to obtain propolis extract D.
The content of flavonoids in each of propolis extracts A1 ', B1 ', C1 ' and D was measured by UV method, and the content of phenolic acid and atorvastatin C in each of propolis extracts was measured by HPLC method, the specific data are shown in Table 1.
TABLE 1 content of flavonoids, phenolic acids and Abirafolin C in each propolis extract
Figure BDA0002340399360000061
According to GB/T24283-2018:
item Cangshen chrysanthemum propolis
Flavonoid/(g/100 g) ≥4.0
Abipilin C/(g/100g) ≥1.4
According to the MTFQ-046 rev03 standard, phenolic acid/(g/100 g) is more than or equal to 5.0. Obviously, the flavonoid, phenolic acid and the atorvastatin C in the propolis extract prepared by the invention are far higher than the standard content. The content of phenolic acid, flavonoid and aliskiren C extracted from the Brazilian ethanol solution has obvious difference, wherein the aliskiren C has the highest content in the propolis extract extracted from the 75% ethanol solution, the phenolic acid has the highest content in the propolis extract extracted from the 85% ethanol solution, and the flavonoid has the highest content in the propolis extract extracted from the 95% ethanol solution, so that the ethanol solutions with different concentrations can be selected to extract the Brazilian ethanol type to obtain the propolis extract with higher content of required components. The propolis extract obtained by mixing and concentrating the filtrate extracted from the three ethanol solutions has higher contents of phenolic acid, flavonoid and atopizin C, and has better comprehensive efficacy.
(2) By using supercritical CO2Extraction method for preparing compound flavone extractF, the specific steps are as follows:
2.1) removing impurities from the ginseng leaves, drying, and crushing the dried ginseng leaves; extracting the propolis extraction residue A in the step 1.4)20、B20、C20Mixing, drying, crushing, mixing with crushed ginseng leaves in equal mass, and sieving with a 18-35 mesh sieve to obtain composite raw material powder;
2.2) adding CO into the composite raw material powder obtained in the step 2.1)2Adding an entrainer absolute ethyl alcohol into a supercritical extractor, performing supercritical extraction at an extraction pressure of 25-35 MPa, a fluid flow rate of 0.5-1 mL/min and an extraction temperature of 40-55 ℃ for 1-3h, and collecting an extract after the extraction is finished to obtain a compound flavone crude extract solution;
2.3) carrying out suction filtration and concentration on the crude extract solution of the compound flavone, diluting the concentrated extract solution with 15-20% ethanol solution, cooling the diluted extract solution for 8-11 hours at the temperature of 3-5 ℃, and carrying out suction filtration again to prepare upper column solution;
2.4) eluting the column loading liquid AB-8 resin column in the step 2.3) by pure water, eluting the resin column by 20-60% ethanol solution, and collecting eluent; concentrating the eluate by rotary evaporation, and vacuum drying to obtain compound flavone extract F.
By using supercritical CO2The extraction method has the advantages of low energy consumption, high flavone yield and low potential safety hazard. Detecting the content of flavonoids in the compound flavone extract F by using a UV method to be 10.49 +/-1.31 (g/100 g); therefore, the content of flavonoids can be effectively improved by adding the ginseng leaves.
(3) Mixing the Brazilian callistemon type propolis extract D, the compound flavone extract F and the beeswax according to a formula ratio, heating, and uniformly stirring to ensure that the components are as follows in parts by weight: 12 parts of Brazilian callistemon herb type propolis extract, 11 parts of compound flavone extract and 3 parts of beeswax;
(4) degassing and defoaming the mixed solution by twice vacuum colloid mills to obtain qualified alcohol chrysanthemum type propolis semi-finished product mixed solution, and keeping the temperature at 45-50 ℃ for later use;
(5) mixing 25 parts of gelatin and 8 parts of glycerol, stirring for 1.5-2h, mixing with 30 parts of purified water, filtering to obtain gelatin solution with certain viscosity and water content, filling the qualified semi-finished product mixed solution of Cangshen chrysanthemum type propolis obtained in step (4) into soft capsules, and performing pelleting, sizing, washing, drying, pill inspection, inner packaging, outer packaging, final inspection and warehousing.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.

Claims (9)

1. A propolis soft capsule of the Brazilian ethanol plant genus type rich in flavone, including capsule shell and capsule content, characterized in that: the capsule comprises the following components in parts by weight: 10-15 parts of Brazilian breynia propolis extract, 9-13 parts of compound flavone extract and 1-5 parts of beeswax;
the capsule shell comprises the following components in parts by weight: 25-30 parts of gelatin, 5-10 parts of glycerol and 25-35 parts of purified water;
the Brazilian breynia type propolis extract is obtained by mixing filtrates obtained by respectively extracting Brazilian breynia type propolis in 75% ethanol solution, 85% ethanol solution and 95% ethanol solution, and concentrating;
the compound flavone extract is prepared by extracting folium Ginseng and Brazilian alcohol type propolis with ethanol to obtain propolis extraction residue, mixing, and extracting with supercritical CO2The extraction method is used for preparation.
2. A method for preparing propolis soft capsules of Brazilian breynia type rich in flavone is characterized in that: the method comprises the following steps:
(1) mixing filtrates obtained by respectively extracting propolis of genus Brazilian wine with 75% ethanol solution, 85% ethanol solution and 95% ethanol solution, and concentrating to obtain propolis extract D of genus Brazilian wine;
(2) mixing folium Ginseng and propolis extraction residue obtained by extracting propolis with ethanol, and supercritical CO2Extracting to obtain compound flavone extract F;
(3) mixing the Brazilian callistemon type propolis extract D, the compound flavone extract F and the beeswax according to a formula ratio, heating, and uniformly stirring to ensure that the components are as follows in parts by weight: the propolis extract is prepared from the following raw materials, by weight, 10-15 parts of Brazilian alcohol-nerium genus propolis extract D, 9-13 parts of compound flavone extract F, and 1-5 parts of beeswax;
(4) degassing and defoaming the mixed solution by twice vacuum colloid mills to obtain qualified alcohol chrysanthemum type propolis semi-finished product mixed solution, and keeping the temperature at 45-50 ℃ for later use;
(5) mixing gelatin and glycerol at a certain ratio, stirring for 1.5-2h, mixing with purified water, filtering to obtain gelatin solution with certain viscosity and water content, filling the qualified semi-finished product mixture of JIUSHENGJU type propolis obtained in step (4) into soft capsule, pressing, shaping, washing, drying, inspecting, packaging, inspecting, and warehousing.
3. The method for preparing propolis soft capsules of the genus Brazilian hop rich in flavones according to claim 2, characterized in that: the preparation method of the Brazilian brevicia propolis extract D comprises the following steps:
1.1) taking a proper amount of Brazilian wine Shen type propolis raw material, and freezing and storing for 16-24 hours at the temperature of-4 to-10 ℃;
1.2) crushing the propolis raw material frozen in the step 1.1) by using a universal crusher for 10-15 minutes, and adding a crushing medium in the crushing process; screening by using a vibrating screen after crushing, wherein the mesh number of the vibrating screen is 40-60 meshes;
1.3) dividing the propolis raw materials screened in the step 1.2) into three equal parts, and marking the three equal parts as a propolis raw material A, a propolis raw material B and a propolis raw material C;
1.4) extracting three equal parts of the propolis raw materials A, B, C in the step 1.3) in three ethanol solutions with different concentrations respectively, wherein the concentration of the ethanol solution is 75-95%, and the specific extraction process is as follows:
1.4.1) preparing the propolis raw material A: ethanol solution E1= 1: adding propolis raw material A into ethanol solution E at a ratio of 6W/V1Leaching for 24 hours at 25 ℃,stirring at regular time and performing ultrasonic enhanced extraction in the extraction process, and collecting propolis extraction residue A after extraction0Pumping the supernatant after the leaching and leaching into a settling tank at the temperature of-6-0 ℃, cooling and settling for 36 hours, filtering the settling liquid by a filter screen with a plate frame of 400 meshes, and collecting the filtered filtrate LA；
1.4.2) according to the propolis raw material B: ethanol solution E2= 1: 6W/V, adding propolis raw material B into ethanol solution E2Extracting at 25 deg.C for 24 hr while stirring and ultrasonic extracting, and collecting propolis residue B0Pumping the supernatant after the leaching and leaching into a settling tank at the temperature of-6-0 ℃, cooling and settling for 36 hours, filtering the settling liquid by a filter screen with a plate frame of 400 meshes, and collecting the filtered filtrate LB；
1.4.3) according to the propolis raw material C: ethanol solution E3= 1: 6W/V, adding propolis material C into ethanol solution E3Extracting at 25 deg.C for 24 hr while stirring and ultrasonic extracting, and collecting propolis residue C0Pumping the supernatant after the leaching and leaching into a settling tank at the temperature of-6-0 ℃, cooling and settling for 36 hours, filtering the settling liquid by a filter screen with a plate frame of 400 meshes, and collecting the filtered filtrate LC；
1.5) the filtrate L obtained in step 1.4)A、LB、LCMixing, and concentrating in a vacuum evaporator to obtain propolis extract D.
4. The method for preparing propolis soft capsules of the genus Brazilian hop rich in flavones according to claim 2 or 3, characterized in that: the preparation method of the compound flavone extract F comprises the following steps:
2.1) removing impurities from the ginseng leaves, drying, and crushing; extracting the propolis extraction residue A in the step 1.4)0、B0And C0Mixing, drying, crushing, mixing with crushed ginseng leaves in equal mass, and sieving with a 18-35 mesh sieve to obtain composite raw material powder;
2.2) compounding the compound obtained in the step 2.1)Adding CO into the powder2Adding an entrainer absolute ethyl alcohol into a supercritical extractor, performing supercritical extraction at an extraction pressure of 25-35 MPa, a fluid flow rate of 0.5-1 mL/min and an extraction temperature of 40-55 ℃ for 1-3h, and collecting an extract after the extraction is finished to obtain a compound flavone crude extract solution;
2.3) carrying out suction filtration and concentration on the crude extract solution of the compound flavone, diluting the concentrated extract solution with 15-20% ethanol solution, cooling the diluted extract solution for 8-11 hours at the temperature of 3-5 ℃, and carrying out suction filtration again to prepare upper column solution;
2.4) eluting the column loading liquid AB-8 resin column in the step 2.3) by pure water, eluting the resin column by 20-60% ethanol solution, and collecting eluent; concentrating the eluate by rotary evaporation, and vacuum drying to obtain compound flavone extract F.
5. The method for preparing propolis soft capsules of the genus Brazilian hop rich in flavones according to claim 3, wherein: the crushing medium is rice hull, rice bran or wheat bran.
6. The method for preparing propolis soft capsules of the genus Brazilian hop rich in flavones according to claim 3, wherein: the ethanol solution E in the step 1.4)1Is 75%, ethanol solution E2Of 85%, ethanol solution E3The concentration of (3) is 95%.
7. The method for preparing propolis soft capsules of the genus Brazilian hop rich in flavones according to claim 3, wherein: in the step 1.4.1), the step 1.4.2) and the step 1.4.3), the regular stirring is performed once every 3 hours for 30min, and the regular stirring speed is 150-200 rpm.
8. The method for preparing propolis soft capsules of the genus Brazilian hop rich in flavones according to claim 3, wherein: in the step 1.4.1), the step 1.4.2) and the step 1.4.3), the ultrasonic wave is strengthened to be ultrasonic once every 4 hours, and the ultrasonic power is 1000W.
9. The method for preparing propolis soft capsules of the genus Brazilian hop rich in flavones according to claim 3, wherein: in the step 1.5), the mixed filtrate is put into a decompression evaporator and heated by adopting water bath, wherein the evaporation temperature is 35-50 ℃, and the vacuum degree is 0.1 MPa.
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