CN107028984B - Propolis gel, propolis gel lyophilized powder, and preparation process and application thereof - Google Patents
Propolis gel, propolis gel lyophilized powder, and preparation process and application thereof Download PDFInfo
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- 241000241413 Propolis Species 0.000 title claims abstract description 149
- 229940069949 propolis Drugs 0.000 title claims abstract description 149
- 239000008176 lyophilized powder Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000000605 extraction Methods 0.000 claims abstract description 58
- 238000000034 method Methods 0.000 claims abstract description 22
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- URFCJEUYXNAHFI-ZDUSSCGKSA-N pinocembrin Chemical compound C1([C@@H]2CC(=O)C3=C(O)C=C(C=C3O2)O)=CC=CC=C1 URFCJEUYXNAHFI-ZDUSSCGKSA-N 0.000 description 1
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- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 235000019633 pungent taste Nutrition 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
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Images
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- 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
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0216—Solid or semisolid forms
- A61K8/022—Powders; Compacted Powders
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/98—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
- A61K8/987—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin of species other than mammals or birds
- A61K8/988—Honey; Royal jelly, Propolis
-
- 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
- A61K9/0012—Galenical forms characterised by the site of application
- A61K9/0019—Injectable compositions; Intramuscular, intravenous, arterial, subcutaneous administration; Compositions to be administered through the skin in an invasive manner
-
- 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
- A61Q17/005—Antimicrobial preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/91—Injection
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- Animal Behavior & Ethology (AREA)
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- Dermatology (AREA)
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Abstract
The invention discloses a propolis gel and a preparation process thereof. The invention also discloses the propolis gel-cleaning lyophilized powder and a preparation process thereof. The preparation process of the invention is stable, the steps are simple, the operation time is short, the requirements on equipment conditions are not high, and compared with the hair glue, the content of the non-fat-soluble propolis extract prepared by the non-critical n-butane extraction step of the process has the yield of propolis net glue of 30-35 percent and the content of total flavonoids of 22-25 percent. The yield of the propolis gel freeze-dried powder is 22.5 to 23.2 percent, and the content of the total flavone is 20 to 25 percent.
Description
Technical Field
The invention belongs to the field of traditional Chinese medicine health care, and particularly relates to propolis gel, propolis gel lyophilized powder, and a preparation process and application thereof.
Background
Propolis is a viscous natural mixture prepared by mixing the resinous material secreted by young buds and callus of plants such as poplar and willow with the secretion of glands such as digestive gland and wax gland (such as beeswax and various digestive enzymes) of bee. Propolis is the effective substance that honeybee was used for maintaining whole colony health, and a bee colony of 5 ~ 6 ten thousand can only produce 100 ~ 150g of propolis in a year, consequently is praised as "purple gold". Propolis is mostly green brown, yellow brown or dark brown, and is solid viscous substance. The product is bitter in taste, irritant, fragrant in resin when burning, viscous and plastic at 35-45 deg.C, soluble as viscous fluid at 65 deg.C, soluble at 100 deg.C, and hard and brittle at 15 deg.C. Propolis is insoluble in water, partially soluble in ethanol, and completely soluble in diethyl ether, chloroform, acetone and benzene. The natural propolis is composed of resin and resin incense compound 39-53 wt%, polyphenol 12-17 wt%, polysaccharide 2-3 wt%, beeswax 19-35 wt%, and impurity (pollen) 8-12 wt%. The known chemical components in various propolis can be more than 300, and the propolis mainly comprises flavonoid compounds such as galangin, pinocembrin and the like. The flavonoids compounds are the main effective components of propolis, and have wide biological activities, such as antioxidant, anti-tumor, anti-inflammatory and immune cell regulating effects.
At present, two main propolis extraction technologies are available, namely organic solvent extraction and supercritical extraction. The propolis components extracted by the organic solvent extraction method are mainly polar components, the dissolution rate of flavonoid compounds is high, the process is simple, the equipment investment is less, but the technical bottlenecks of low flavone content, high heavy metal content, solvent residue, thick color of extracted products, low extraction efficiency, long production period and the like caused by incomplete extraction exist in the extracted products. The supercritical CO2 extraction of propolis has low operation temperature (31 deg.C), and can complete the whole extraction and separation operation at room temperature to prevent active components from being damaged; in the whole extraction process, the propolis is less in contact with air, so that the extracted active ingredients can be prevented from being oxidized; can effectively remove heavy metals such as lead and the like in the propolis raw material; the extraction process has the advantages of simple flow, few steps, short extraction time, short production period and the like. However, in the supercritical CO2 fluid extraction process, the extraction pressure and temperature, the separation pressure and temperature, the fluid flow and extraction time, the entrainer type and the addition amount are important factors influencing the extraction rate and the biological activity of the active ingredients, and the extraction rate of the propolis extract is reduced along with the increase of the operation temperature; the pressure and the flow rate of the carbon dioxide are increased continuously, but the pressure and the flow rate show a descending trend at high pressure and high flow rate. Compared with alcohol extraction propolis, the supercritical fluid extract of the propolis has lower flavone content, and the flavonoid compound is one of the main components of the propolis having the anti-oxidation effect, so that the anti-oxidation effect of the supercritical fluid extract of the propolis is not obvious, and the activity of the supercritical fluid extract of the propolis is not purely and positively correlated with the flavone content.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to solve the technical problem of providing a preparation process of propolis gel.
The invention also aims to solve the technical problem of providing a preparation process of the propolis gel lyophilized powder. The invention adopts non-critical low-temperature fluid extraction technology to prepare propolis. The method combines the advantages of alcohol extraction and carbon dioxide supercritical extraction of propolis, solves the disadvantages of propolis extraction method, and the prepared propolis contains no alcohol component, does not change the properties of propolis, has high active ingredient content, and strong pungent taste; and the residual quantity of the extraction solvent is 1ppm and is far lower than the national standard of 50 ppm.
The invention finally solves the technical problem of providing the application of the propolis gel and the propolis gel lyophilized powder.
The technical scheme is as follows: in order to solve the technical problems, the technical scheme adopted by the invention is as follows: a preparation process of propolis gel comprises the following steps:
1) pretreatment: collecting Brazilian green propolis, precooling, crushing, and collecting propolis particles;
2) mixing: mixing the pretreated propolis particles with rice hulls in a ratio of 1: 1-8 to obtain a mixture;
3) non-critical fluid extraction: adding n-butane into the mixture, and extracting in an extraction tank at the extraction pressure of 1-10 MPa, the temperature of 20-50 ℃ and the stirring speed of 30-40 rpm; standing for 30-60 min to obtain n-butane extract;
4) solid-liquid separation: conveying the n-butane extract to an evaporation tank for evaporation, wherein propolis gel and rice hulls with the propolis gel are left in the extraction tank;
5) screening: and (4) screening the propolis gel and the rice hulls with the propolis gel by using a 20-100-mesh sieve to obtain the propolis gel.
Wherein the pre-cooling temperature in the step 1) is-5 ℃ to-20 ℃, and the pre-cooling time is 5-20 hours.
Wherein the extraction pressure in the step 3) is 6MPa and the extraction temperature is 40 ℃.
The propolis gel is prepared by the preparation process.
A preparation process of propolis gel lyophilized powder comprises the following steps:
1) soaking: adding the rice hulls with the propolis neat gel obtained in the step 5) of any one of claims 1-3 into 95% edible-grade ethanol according to a solid-liquid ratio of 1: 5-8, stirring at the same time, and soaking for 12-16 hours at a stirring speed of 30-40 rpm to obtain a solid-liquid mixture;
2) solid-liquid separation: sieving the solid-liquid mixture by using a 80-mesh screen, removing rice hulls, collecting, leaving supernatant in an extraction tank, standing for 4-6 hours, heating the supernatant to obtain a semi-fluid extract, and recovering edible ethanol at the same time;
3) and (3) freeze drying: vacuum freeze-drying the semi-fluid extract to obtain the propolis gel lyophilized powder particles, which are divided into three stages: pre-cooling, freezing and heating; the pre-cooling temperature is-18 ℃ to-20 ℃, and the night is kept; the temperature of the cold trap in the freezing treatment process is-26 ℃, the freezing time is 18-20 hours, the sublimation temperature in the heating treatment process is 40-45 ℃, and the sublimation time is 14-16 hours; the vacuum degree in the whole vacuum drying process is-0.9 to-0.1 MPa;
4) crushing and screening: sieving the propolis gel lyophilized powder particles with a 80-mesh sieve, and sieving to obtain the propolis gel lyophilized powder.
Wherein the heating temperature in the step 2) is 50-55 ℃.
Wherein, the pressure in the extraction tank in the step 2) is-0.9 to-0.1 MPa.
The invention also comprises the propolis gel lyophilized powder prepared by the process.
The invention also comprises the application of the propolis gel or the propolis gel lyophilized powder in the preparation of medicines, foods and daily chemical products. The propolis gel and propolis gel lyophilized powder has the effects of resisting bacteria, diminishing inflammation, relieving itching, resisting oxidation, enhancing immunity, reducing blood sugar, reducing blood fat and the like, and is mainly used in the industries of medicine, food, daily chemical industry and the like.
Has the advantages that: the invention adopts an extraction technology that low-temperature non-critical fluid n-butane is used as a solvent, uses baxi A-grade green propolis feather glue as a raw material, and prepares propolis particles through the main steps of sorting, freezing at-10 ℃, crushing, blending with rice hulls, extracting by using non-critical fluid, screening, freeze drying, crushing, packaging and the like. The invention aims to improve the extraction yield, flavone content and biological activity of the Brazilian green propolis clean gel and reduce solvent residue on the premise of not changing the physical properties, color, special taste and the like of raw materials. The preparation process of the invention is stable, the steps are simple, the operation time is short, the requirements on equipment conditions are not high, and compared with the hair glue, the content of the non-fat-soluble propolis extract prepared by the non-critical n-butane extraction step of the process has the yield of propolis net glue of 30-35 percent and the content of total flavonoids of 22-25 percent. The yield of the propolis gel freeze-dried powder is 22.5 to 23.2 percent, and the content of the total flavone is 20 to 25 percent.
Drawings
FIG. 1 is a flow chart of a preparation process of propolis gel;
FIG. 2 is a flow chart of the preparation process of propolis gel lyophilized powder.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available. The Brazilian green propolis is purchased from MN Pr pol is company.
The yield of the propolis neat gel is calculated according to the following formula:
the yield of the propolis neat gel is equal to the weight of the propolis neat gel/the weight of the propolis crude gel is 100
The yield of the semi-fluid extract before freeze-drying is calculated according to the following formula:
yield of semi-fluid extract before freeze-drying is equal to weight of semi-fluid extract before freeze-drying/weight of rice husk with propolis pure gum is 100
The yield of the propolis gel-removing freeze-dried powder is calculated according to the following formula:
the yield of the propolis gel lyophilized powder is equal to the weight of the propolis gel lyophilized powder/the weight of the semi-fluid extract before lyophilization is 100
Example 1 preparation of propolis gel
A preparation process of propolis gel comprises the following steps:
1) pretreatment: collecting 165kg of Brazilian green propolis raw gum, carrying out precooling treatment at the temperature of minus 10 ℃ for 12 hours, and then carrying out crushing treatment to obtain propolis particles;
2) mixing: mixing the pretreated propolis particles with rice hulls in a ratio of 1: 4 to obtain a mixture;
3) non-critical fluid extraction: adding n-butane into the mixture, and extracting in an extraction tank at the extraction pressure of 6MPa, the temperature of 40 ℃ and the stirring speed of 30 rpm; standing for 60min to obtain n-butane extract;
4) solid-liquid separation: conveying the n-butane extract to an evaporation tank for evaporation, wherein propolis gel and rice hulls with the propolis gel are left in the extraction tank;
5) screening: sieving propolis gel and rice hull with 80 mesh sieve to obtain 49.5kg propolis gel.
Example 2 preparation of propolis gel
A preparation process of propolis gel comprises the following steps:
1) pretreatment: collecting 165kg of Brazilian green propolis raw gum, carrying out precooling treatment at the temperature of minus 5 ℃ for 20 hours, and then carrying out crushing treatment to obtain propolis particles;
2) mixing: mixing the pretreated propolis particles with rice hulls in a ratio of 1: 1 to obtain a mixture;
3) non-critical fluid extraction: adding n-butane into the mixture, and extracting in an extraction tank at the extraction pressure of 1MPa, the temperature of 50 ℃ and the stirring speed of 40 rpm; standing for 30min to obtain n-butane extract;
4) solid-liquid separation: conveying the n-butane extract to an evaporation tank for evaporation, wherein propolis gel and rice hulls with the propolis gel are left in the extraction tank;
5) screening: sieving propolis gel and rice hull with 20 mesh sieve to obtain 54.45kg propolis gel.
Example 3 preparation of propolis gel
A preparation process of propolis gel comprises the following steps:
1) pretreatment: collecting 165kg of Brazilian green propolis raw gum, carrying out precooling treatment at the temperature of minus 20 ℃ for 5 hours, and then carrying out crushing treatment to obtain propolis particles;
2) mixing: mixing the pretreated propolis particles with rice hulls in a ratio of 1:8 to obtain a mixture;
3) non-critical fluid extraction: adding n-butane into the mixture, and extracting in an extraction tank at the extraction pressure of 10MPa, the temperature of 20 ℃ and the stirring speed of 35 rpm; standing for 45min to obtain n-butane extract;
4) solid-liquid separation: conveying the n-butane extract to an evaporation tank for evaporation, wherein propolis gel and rice hulls with the propolis gel are left in the extraction tank;
5) screening: sieving propolis gel and rice hull with 100 mesh sieve to obtain 57.75kg propolis gel.
EXAMPLE 4 preparation of propolis gel-free lyophilized powder
1) Soaking: adding the rice hulls with the propolis neat gel obtained in the step 5) of the embodiment 1 into 95% edible ethanol according to the solid-liquid ratio of 1:5, stirring at the same time, soaking for 12 hours, and stirring at the speed of 40rpm to obtain a solid-liquid mixture;
2) solid-liquid separation: sieving the solid-liquid mixture by using a 80-mesh screen, removing rice hulls, collecting, leaving supernatant in an extraction tank, standing for 4-6 hours, heating the supernatant to obtain 75kg of semi-fluid extract, and recovering edible ethanol at the same time; the heating temperature is 50 ℃; the pressure in the extraction tank is-0.1 MPa;
3) and (3) freeze drying: vacuum freeze-drying the semi-fluid extract to obtain the propolis gel lyophilized powder particles, which are divided into three stages: pre-cooling, freezing and heating; the pre-cooling temperature is-18 ℃ and is kept overnight; the temperature of the cold trap in the freezing treatment process is-26 ℃, the freezing time is 18h, the sublimation temperature in the heating treatment process is 40 ℃, and the sublimation time is 14 h; the vacuum degree in the whole vacuum drying process is-0.1 MPa;
4) crushing and screening: the propolis gel lyophilized powder particles are sieved by a 80-mesh sieve, and the propolis gel lyophilized powder is sieved to obtain 16.9 kg.
EXAMPLE 5 preparation of propolis gel-free lyophilized powder
1) Soaking: adding the rice hulls with the propolis neat gel obtained in the step 5) of the embodiment 2 into 95% edible ethanol according to the solid-liquid ratio of 1:8, stirring at the same time, soaking for 16 hours, and stirring at the speed of 30rpm to obtain a solid-liquid mixture;
2) solid-liquid separation: sieving the solid-liquid mixture by using a 80-mesh screen, removing rice hulls, collecting, leaving supernatant in an extraction tank, standing for 4-6 hours, heating the supernatant to obtain 69kg of semi-fluid extract, and recovering edible ethanol at the same time; the heating temperature is 55 ℃; the pressure in the extraction tank is-0.9 MPa.
3) And (3) freeze drying: vacuum freeze-drying the semi-fluid extract to obtain the propolis gel lyophilized powder particles, which are divided into three stages: pre-cooling, freezing and heating; the pre-cooling temperature is-20 ℃, and the night is kept; the temperature of the cold trap in the freezing treatment process is-26 ℃, the freezing time is 20h, the sublimation temperature in the heating treatment process is 45 ℃, and the sublimation time is 16 h; the vacuum degree in the whole vacuum drying process is-0.9 MPa;
4) crushing and screening: the propolis gel lyophilized powder particles are sieved by a 80-mesh sieve, and the propolis gel lyophilized powder is sieved to obtain 16.6 kg.
Example 6 preparation of propolis lyophilized powder
1) Soaking: adding the rice hulls with the propolis neat gel obtained in the step 5) of the embodiment 3 into 95% edible ethanol according to the solid-liquid ratio of 1:6, stirring at the same time, soaking for 14 hours, and stirring at the speed of 35rpm to obtain a solid-liquid mixture;
2) solid-liquid separation: sieving the solid-liquid mixture by using a 80-mesh screen, removing rice hulls, collecting, leaving supernatant in an extraction tank, standing for 4-6 hours, heating the supernatant to obtain 68kg of semi-fluid extract, and recovering edible ethanol at the same time; the heating temperature is 53 ℃; the pressure in the extraction tank is-0.5 MPa;
3) and (3) freeze drying: vacuum freeze-drying the semi-fluid extract to obtain the propolis gel lyophilized powder particles, which are divided into three stages: pre-cooling, freezing and heating; the pre-cooling temperature is-19 ℃, and the night is kept; the temperature of the cold trap in the freezing treatment process is-26 ℃, the freezing time is 19h, the sublimation temperature in the heating treatment process is 43 ℃, and the sublimation time is 15 h; the vacuum degree in the whole vacuum drying process is-0.5 MPa;
4) crushing and screening: sieving the propolis gel lyophilized powder particles with a 80-mesh sieve to obtain 15.8kg of propolis gel lyophilized powder.
Experimental example 1
The yield and the total flavone content of the propolis neat gel prepared in the embodiment 1-3 are respectively measured by the method; the yield of the semi-fluid extract before freeze-drying, the yield of the propolis gel freeze-dried powder and the content of total flavonoids, which are prepared in the embodiments 4-6, are respectively measured:
the results are shown in Table 1:
experimental example 2 clinical experimental verification of propolis gel and propolis gel lyophilized powder
1. In the experimental example, the propolis gel prepared in the examples 1 to 3 is adopted to carry out experimental verification on a diabetic patient and a hyperlipoidemia patient respectively, and the experimental results of the blood sugar content before meals of the diabetic patient after 16 weeks and 16 weeks are shown in table 2, and the experimental results of the blood fat content of the hyperlipoidemia patient are shown in table 3;
TABLE 2
TABLE 3
2. In the experimental example, the propolis gel lyophilized powder prepared in examples 4 to 6 is used for experimental verification of a diabetic patient and a hyperlipidemic patient respectively, and the experimental results of the pre-meal blood sugar content of the diabetic patient after 12 weeks are shown in table 4 and the blood fat content of the hyperlipidemic patient is shown in table 5, wherein the experimental results of the pre-meal blood sugar content of the diabetic patient after 12 weeks are observed at the same time;
TABLE 4
TABLE 5
Two specific cases are listed below:
case 1
Mabaojun, male, 63 years old, suffered from diabetes for many years, had a blood sugar index of 8.25 mmol/L before meal, and had a blood sugar index reduced to 6.3 mmol/L after 16 weeks of administration of the propolis gel prepared in example 1, and blood sugar had recovered to a normal value at present.
Case 2
The blood fat index of the propolis gel dry powder prepared in the example 4 is reduced to 3.5 mmol/L after 12 weeks, which is stable and normal when the propolis gel dry powder is taken for the men in the age of 61 years and the blood fat is 6.6 mmol/L.
While specific embodiments of the invention have been described in detail, those skilled in the art will understand that. Various modifications and alterations of those details may be made in light of the overall teachings of the disclosure, and are within the scope of the invention. The full scope of the invention is given by the appended patent claims and any equivalents thereof.
Claims (2)
1. The preparation method of the propolis gel is characterized by comprising the following steps:
1) pretreatment: collecting Brazilian green propolis, precooling, crushing, and collecting propolis particles; the pre-cooling temperature is-10 ℃, and the pre-cooling time is 12 hours;
2) mixing: mixing the pretreated propolis particles with rice hulls in a ratio of 1: 4 to obtain a mixture;
3) non-critical fluid extraction: adding n-butane into the mixture, and extracting in an extraction tank at the extraction pressure of 6MPa, the temperature of 40 ℃ and the stirring speed of 30 rpm; standing for 60min to obtain n-butane extract;
4) solid-liquid separation: conveying the n-butane extract to an evaporation tank for evaporation, wherein propolis gel and rice hulls with the propolis gel are left in the extraction tank;
5) screening: sieving propolis gel and rice hull with 80 mesh sieve to obtain propolis gel.
2. The preparation method of the propolis gel lyophilized powder is characterized by comprising the following steps:
1) pretreatment: collecting Brazilian green propolis, precooling, crushing, and collecting propolis particles; the pre-cooling temperature is-10 ℃, and the pre-cooling time is 12 hours;
2) mixing: mixing the pretreated propolis particles with rice hulls in a ratio of 1: 4 to obtain a mixture;
3) non-critical fluid extraction: adding n-butane into the mixture, and extracting in an extraction tank at the extraction pressure of 6MPa, the temperature of 40 ℃ and the stirring speed of 30 rpm; standing for 60min to obtain n-butane extract;
4) solid-liquid separation: conveying the n-butane extract to an evaporation tank for evaporation, wherein propolis gel and rice hulls with the propolis gel are left in the extraction tank;
5) screening: sieving propolis gel and rice hull with propolis gel with 80 mesh sieve to obtain propolis gel;
6) soaking: adding the rice hulls with the propolis neat gel obtained in the step 5) into 95% edible ethanol according to the solid-liquid ratio of 1:5, simultaneously stirring, soaking for 12 hours, and stirring at the speed of 40rpm to obtain a solid-liquid mixture;
7) solid-liquid separation: sieving the solid-liquid mixture by using a 80-mesh screen, removing rice hulls, collecting, leaving supernatant in an extraction tank, standing for 4-6 hours, heating the supernatant to obtain a semi-fluid extract, and recovering edible ethanol at the same time; the heating temperature is 50 ℃; the pressure in the extraction tank is-0.1 MPa;
8) and (3) freeze drying: vacuum freeze-drying the semi-fluid extract to obtain the propolis gel lyophilized powder particles, which are divided into three stages: pre-cooling, freezing and heating; the pre-cooling temperature is-18 ℃ to-20 ℃, and the night is kept; the temperature of the cold trap in the freezing treatment process is-26 ℃, the freezing time is 18-20 hours, the sublimation temperature in the heating treatment process is 40-45 ℃, and the sublimation time is 14-16 hours; the vacuum degree in the whole vacuum drying process is-0.1 MPa;
9) crushing and screening: sieving the propolis gel lyophilized powder particles with a 80-mesh sieve, and sieving to obtain the propolis gel lyophilized powder.
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| CN101161324A (en) * | 2006-10-11 | 2008-04-16 | 韩延欣 | Sub-critical fluid extraction solvent and abstraction method |
| CN101530178A (en) * | 2009-04-16 | 2009-09-16 | 江苏江大源生态生物科技有限公司 | Method for extracting propolis by simulative biological fluid bed supercritical CO2 fluid |
| CN104522451A (en) * | 2015-02-03 | 2015-04-22 | 芜湖蜂联有限公司 | Method for purifying propolis liquid |
| CN106074617A (en) * | 2016-08-24 | 2016-11-09 | 深圳市荣格保健品有限公司 | A kind of propolis extract and extraction process thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101161324A (en) * | 2006-10-11 | 2008-04-16 | 韩延欣 | Sub-critical fluid extraction solvent and abstraction method |
| CN101530178A (en) * | 2009-04-16 | 2009-09-16 | 江苏江大源生态生物科技有限公司 | Method for extracting propolis by simulative biological fluid bed supercritical CO2 fluid |
| CN104522451A (en) * | 2015-02-03 | 2015-04-22 | 芜湖蜂联有限公司 | Method for purifying propolis liquid |
| CN106074617A (en) * | 2016-08-24 | 2016-11-09 | 深圳市荣格保健品有限公司 | A kind of propolis extract and extraction process thereof |
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