CN1220497C - Antivirus antioxidizing active extract of proplis and its molecular inclusion compound - Google Patents

Antivirus antioxidizing active extract of proplis and its molecular inclusion compound Download PDF

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CN1220497C
CN1220497C CNB011417633A CN01141763A CN1220497C CN 1220497 C CN1220497 C CN 1220497C CN B011417633 A CNB011417633 A CN B011417633A CN 01141763 A CN01141763 A CN 01141763A CN 1220497 C CN1220497 C CN 1220497C
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propolis
powder
deleading
purification
extract
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CN1342464A (en
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姜德勇
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Abstract

The present invention discloses an antivirus antioxidizing active extract of propolis, purified lead removing propolis powder, and a manufacture method thereof. Through the improvements of the technical skill of raw material pretreatment, dissolvent extraction, filtration and drying in the process of purifying propolis, the purity of the antivirus antioxidizing active extract of propolis and the total flavone content of propolis are improved, and the novel technical skill of five kinds of removal, such as propolis hyposensitization, heavy metal lead removal, etc., is innovated. The present invention also discloses a group of propolis food and health food, and particularly relates to novel preparations, which has a targeting property and a slow control release property, such as molecular clathrate, micro capsules, microballoons, nanoparticles, etc., and manufacture methods thereof.

Description

Propolis antivirus antioxidizing active extract and molecular clathrate preparation thereof
Technical field
The present invention relates to the propolis health-care products that a kind of propolis extracting method and this method products therefrom thereof make.
Background technology
The source of propolis, characteristics, the biological property that Main Ingredients and Appearance and Apis thereof are gathered propolis all has introduction in following known technology: (Shanxi science tech publishing house publishes " propolis ", pillars of a house chief editor, January in 1999 the 1st edition, the 1-19 page or leaf), " the surprising drug effect of propolis " (Taiwan justice publishing house, July in 1992 the 1st edition, numerous professor Tai Lang chief editor under the clear and medical university's wood of Japan, the Liu Xueqing translation, the 20-42 page or leaf), (Paris, FRA Librairie Maloine S.A.Editeur publishes " Propolisin Natural Therpeutics ", nineteen eighty-three the 2nd revised edition, the 20-28 page or leaf) and " プ ロ Port リ ス そ drug effect The visit Ru " (Chinese " drug efficacy study of propolis " by name, リ ョ Application society publishes, March in 1994 the 1st edition, Song Yezhe also writes).
Propolis (Propolis) is that Apis is gathered extraneous plant sprout bud and secreted natural gum (Gum), resin (Resin), balsam (Balsam) and the oleoresin resinoids such as (Oil-resin) in trunk wound, and sneaks into Apis salivary gland secretion (sialic acid Saliva acid and ptyalin Saliva enzyme) and the formed a kind of yellowish-brown jelly of Cera Flava (Wax).
Propolis derives from the secretions of plant.The first is after plant comes to harm or poisons, just secrete a kind of yellowish-brown jelly from epidermis, this jelly is the pathological product of plant, mainly be to be used for protective plant to exempt from injury, wherein mainly be the bigger complicated pluralism phenolic compound (Phytoncide) of natural gum, resin, volatile oil, tannin (Tannin) and molecule, these materials can be that insoluble matter is used to suppress the infringement to plant such as antibacterial and virus with protein bound; It two is plant tree bud, leaves and the normal resinae secretions of trunk epidermis.The physiology product that these two kinds of secretions all are plant metabolisms has the complex physical effect, is that plant adapts to natural biological nature.
Owing to contain many aromatics volatile matters in the propolis and have the polyphenols of maximum absorption band at ultraviolet region, therefore, Apis is gathered propolis and is not only in order to fill up slit in the Nidus Vespae, prevent the invasion of disease harmful animal, and be the stimulant (attractant) of a kind of bee gathering and visual activity, be that Apis adapts to natural a kind of biological nature.
The inventor concentrates on studies for many years, test and analytical test are learnt, are to contain multiple active substance composition with special pharmacological drug action in the bee glue purifying of raw material production with Chinese propolis: wherein mainly comprise propolis flavone (Propolis Flavonoids), propolis lignanoid (Propolis Lignin), propolis coumarin (PropolisCoumarins), propolis lactone (Propolis Lactone), propolis anthraquinone (Propolis Anthraguinone), propolis stilbene class (Propolis Stilbene), propolis Saponin (Propolis Saponins), propolis volatile oil (Propolis Oils), propolis organic acid (Propolis Organic acis) and propolis terpenoid nearly thousand kinds of active substance compositions of ten big classes such as (Propolis Terpenoides).Be described as by medical expert " natural plants explosive component treasure-house ", claim that Apis is " magical medical expert ".
The pharmacology and the drug action of propolis mainly contain: 1. antibacterial action.The propolis tool is wanted the antibacterial and bactericidal action of broad-spectrum, and antibiotics is had obvious synergistic effect; 2. blood circulation promoting and blood stasis dispelling, anti-inflammatory and antalgic, antiulcer action; 3. antioxidation and antifatigue effect; 4. antiviral, protect the liver and improve the gastrointestinal function effect; 5. resisiting influenza virus effect; 6. hypoglycemic activity; 7. vessel softening and effect for reducing blood fat; 8. hypotensive activity; 9. immunostimulant, slow down aging, microcirculation improvement and antitumaous effect; 10. local anesthesia and promotion tissue regeneration effect.Propolis has peculiar prevention and therapeutical effect to human numerous disease, can be used for treatment: 1. dermatosis: eczema, acne, verruca plana, psoriasis and beriberi etc.; 2. ear,nose ﹠ throat disease; 3. oral disease; 4. internal disease: gastric and duodenal ulcers disease, chronic enteritis, hepatitis, respiratory organ disease, hyperlipemia and blood high viscosity syndrome; 5. prevent and treat diabetes, hypertension and heart disease, cardiovascular and cerebrovascular disease; 6. surgical diseases: sterilization, pain relieving, treatment are burnt, chronic ulcer, hyperosteogeny, osteoporosis, rheumatic and atrophic arthritis and damage, anus etc.; 7. other disease: tinea unguium, gynaecopathia, ophthalmic diseases, tuberculosis; 8. antitumor is as prevention and auxiliary treatment nasopharyngeal carcinoma, breast carcinoma and leukemia etc.
In the active substance composition of the above-mentioned multiple special pharmacological drug action that contains, that propolis the most important thing is is antibiotic, antiviral, biological antioxidant and anti-tumor activity composition.
The propolis active substance composition that contains 35-45% in the raw material propolis approximately is a bee glue purifying, other 55-65% is an insoluble impurities, mainly contains 1. Cera Flava, ethanol insoluble resin and some insoluble impuritiess such as wood flour, residual broken Apis body, wire gauze disintegrating slag, iron nail, fine earth slag, fine sand and crushed stone etc.; 2. the nonactive composition of hot ethanol soluble resin class; 3. heavy metal pollution (as lead, hydrargyrum and arsenic etc.); 4. agricultural residual pollution; 5. main sensitizer.
At present, it mostly is edible ethanol and the heating extraction of taking the 70-90% variable concentrations that the purification of propolis is both at home and abroad produced, filter method is simple coarse also, make and contain insoluble impurities and harmful heavy metal etc. in the final propolis extract, thereby make effective component content contained in the propolis on the low side relatively.Therefore, existing propolis extraction process still has many weak points:
(1) extracts temperature drift: extract temperature generally at 55-65 ℃, dissolved the extracting of the nonactive composition of resinae of a small amount of Cera Flava and some solubilities will be arranged like this; 2. filtering accuracy is low: filter method generally is to filter with 200 order metal screens; Or earlier with 80 order gauze coarse filtration, reuse 300 order gauze filter pressings; 3. it is low to extract solvent strength: the edible ethanol that mainly is to use the 70-90% variable concentrations; 4. the ratio of extracting solvent and propolis raw material is little: generally be 1.5 to 1; 5. still contain a small amount of Cera Flava and insoluble impurities; 6. contain soluble impurity; 7. heavy metal and agricultural residual pollution are arranged; 8. unresolved propolis allergic problem; 9. thoroughly do not solve the agricultural technology problem of full component water-soluble bee glue: the preparation method of water-soluble bee glue is directly to carry out processing with the raw material propolis at present.Should be purification deleading, desensitization and the purified technology production technology problem thereof that solves the raw material propolis earlier, on the basis of bee glue purifying, the reuse dissolution with solvents prepares water-soluble bee glue then.
Ah he's wound of Amada Co., Ltd.'s woods protobiochemistry institute waits at Chinese patents CN1194967A " has the water miscible propolis extract of improvement ": it is characterized in that preparation propolis extractive with organic solvent earlier, extract with the solvent that contains alkali or basic anhydride of PH between 5-7 then, propolis composition in the prepared propolis water solubility extract remains the water-soluble bee glue extract of propolis-containing part component, is not full component water-soluble bee glue extract.Name is called to have disclosed in No. 00105486.4 Chinese patent application of " processing art for extracting propolis and removing lead from it " a kind ofly " to be pulverized propolis after below-4 ℃ freezing 12 hours through liquid nitrogen cryogenics; The variable concentrations edible ethanol is merceration repeatedly; Filtering lead is got rid of in freezing sedimentation under the critical state; Binodal energy vacuum and low temperature concentrating under reduced pressure; A kind of processing art for extracting propolis and removing lead from it that the method that alcohol distillation column distillation recovery alcohol in high concentration utilizes is again finished." not only deleading is incomplete in this patent application, and mentions for not giving such as the removal of hydrargyrum, arsenic one class poisonous metal, do not give equally for the removal of the removal of residual pesticide and heat-sensitive materials relating to.
Therefore, existing propolis purifying technique is anxious waits to improve.
In sum, the application of propolis at first will solve the purification of propolis raw material and remove heavy metal lead, desensitization etc., the propolis Patent document data of nearly by retrieval 40 years (after 1962) domestic and international more or less a hundred countries, in conclusive evidence propolis purification technique and the production technology, also do not solve simultaneously and remove five purification technique that takes off and production technologies such as heavy metal lead and desensitization.
Summary of the invention
---the invention provides a kind of preparation method of pure deleading propolis powder and the health preparation of the propolis powder system that makes by this method.It has improved pre-treatment, solvent extraction, filtration and the drying technique of raw material in the propolis purification process preparation method provided by the invention, thereby has improved the purity of propolis antivirus antioxidizing active extract and the content of propolis total flavones; And provide in the propolis purification process purify Cera Flava and insoluble impurities, remove organochlorine pesticide residual, desensitize, remove such as a class heavy metal such as lead and hydrargyrum and the nonactive composition of resinae etc. five that removes some solubilities and take off technology.
---in the manufacture method of purification deleading propolis powder provided by the invention, comprising: 1. the raw material propolis is being higher than pre-freeze under-4 ℃-0 ℃ the condition; 2. the raw material propolis after the pre-freeze is crushed to 40 orders or thinner powder rapidly with common beater grinder; 3. then raw material propolis powder is joined lentamente being equipped with in the propolis extraction pot that extracts solvent of stirring; 4. extracting solvent is 95% (or more than 95%) edible ethanol or dehydrated alcohol; 5. raw material propolis powder and the ratio of extracting solvent are 1 than 3.5-4.5 (W/W); 6. mixing speed is 8-15 rev/min; 7. extracting temperature is normal temperature laboratory; 8. extraction time is 8-12 hour; 9. filter type adopts micropore fine filtration technology to make with extra care filtration; 10. concentrate and reclaim solvent and drying under reduced pressure, pulverize after cooling is placed and promptly get the deleading propolis powder of purifying.Finally make the purity of propolis antivirus antioxidizing active extract reach 100%, solid content reaches more than 99.9%; Content of heavy metal lead≤0.01ppm, the content of propolis total flavones reaches (wherein three kinds of flavone sums of pinocembrin Pinocembrin, chrysin Chrysin and galangin Galangin reach more than 8%, adopt high performance liquid chromatography-HPLC test) more than 10%.
---in the manufacture method of purification deleading propolis powder provided by the invention, disclosed the propolis purification process, comprise: 1. purify Cera Flava and insoluble impurities: selection concentration is that edible ethanol or the dehydrated alcohol more than 95% or 95% made the extraction solvent, and under the condition of normal temperature laboratory, stir extraction, be that the micropore fine filtration technology of 100 nanometers is made with extra care filtration finally with the aperture; 2. it is residual to remove organochlorine pesticide: adopt the adsorbent resin that chlorinated organics is had a selective absorption that organochlorine pesticide is carried out selective absorption and remove; 3. desensitization: purify insoluble impurities, extract at room temperature to remove the hot ethanol soluble substance and to adopt adsorbent to carry out the adsorbing and removing sensitizer; 4. remove such as plumbous and hydrargyrum one class heavy metal: adopt ion exchange resin that heavy metal is had a selective absorption to as plumbous and hydrargyrum one class heavy metal reach and carry out selective absorption as arsenic one class harmful element and remove; 5. remove the nonactive composition of resinae of some solubilities: extract at room temperature is with the nonactive composition of resinae of the solubility of removing the hot ethanol stripping, is that the micropore fine filtration technology of 100 nanometers is made with extra care filtration with the aperture finally.
---the deleading propolis powder that the invention provides the method purification that discloses with the present invention is the health food containing propolis that primary raw material is made, the content range of deleading propolis powder of wherein purifying is 10-100%, the content range of additive is 0-90%, additive is respectively: Lac regis apis dry powder, bee pollen, broker wall bee pollen and extract thereof, queen bee embryo (larva) dry powder and extract thereof, Nidus Vespae and extract thereof, the pupa albumen extract, Pollen Typhae pollen, breaking cellular wall Pollen Typhae pollen and extract thereof, Pollen Pini, breaking cellular wall Pollen Pini and extract thereof, oatmeal and extract thereof, Fructus Cucurbitae moschatae powder and extract thereof, juice powder, the vegetable juice powder, Se-rich xianggu powder and extract thereof, health must selenium powder, selenium-enriched edible mushroom powder and extract thereof, smart powder of Ganoderma herb and ganoderan extract thereof, Ganoderma spore powder, Ganoderma spore powder with cellular wall broken and extract thereof, biological calcium powder, vitamin A, the vitamin B powder, vitamin c powder, vitamin D powder, vitamin E, other vitamin, the compound vitamin powder, ginkgo leaf extract powder and Folium Ginkgo flavone extract thereof, smart powder of Folium Kaki and Folium Kaki flavone extract thereof, be medicine be again the natural animal-plant activity extract of food, panax ginseng extractum powder and extract thereof, Radix Panacis Quinquefolii and red sage root refined powder and extract thereof, natural Chinese medicinal herb vegetable active extract, lactose, dextrin, α, beta, gamma-cyclodextrin and derivant thereof, maltodextrin, starch, superfine SiO 2, magnesium hydroxide, calcium carbonate, mannitol, xylitol, microcrystalline Cellulose, polyvinylpyrrolidone, Polyethyleneglyeol, polyoxyethylene (40) monostearate (S-40), Poloxamer 188, gelatin, stearic acid, sodium stearate etc. or its compositions.
---it is the health food containing propolis that raw material is made that the present invention also provides the purification deleading propolis powder that makes with described method, and described health product are confection, chewing gum, chewing gum, such as dosage forms such as buccal tablet and effervescent tablet one class tablet, capsule, granule, instant and drop pill.
---what the invention provides that described method makes is the health product that raw material is made with purification deleading propolis powder, described health product just like: 1. selenium spirit bee glue powder capsule: deleading propolis powder 20-50% wherein purifies, Ganoderma spore powder with cellular wall broken 20-25%, selenium-enriched edible mushroom powder or health must selenium powder 20-25%, cyclodextrin 0-40%; 2. bee glue powder capsule, the deleading propolis powder 75-100% that wherein purifies, cyclodextrin 0-25% or polyvinylpyrrolidone 0-25% or superfine SiO 2 0-25%; 3. the outstanding capsule of propolis ganoderma lucidum, 50 parts of weight of Ganoderma spore powder with cellular wall broken wherein, 25 parts of weight of purification deleading propolis powder, 25 parts of weight of cyclodextrin, 20 parts of weight of queen bee embryo dry powder; 4. the compound extraordinary bee pollen electuary of propolis, the deleading propolis powder 10% of wherein purifying, bee pollen 50-90%, other additive 0-40%.
---what the invention provides that described method makes is the health product that having of raw material manufacturing improved sleep and chemical liver injury had the health-care effect of auxiliary protection with purification deleading propolis powder; described health product are selenium spirit bee glue powder capsule; deleading propolis powder 20-50% wherein purifies; Ganoderma spore powder with cellular wall broken 20-25%; selenium-enriched edible mushroom powder (health must selenium powder) 20-25%, cyclodextrin 0-40%.
---what the invention provides that described method makes is the auxiliary health product that suppress the health-care effect of tumor of having of raw material manufacturing with purification deleading propolis powder, described health product are honeybee Lingbao City capsule, wherein Ganoderma spore powder with cellular wall broken 50%, purification deleading propolis powder 25%, broker wall bee pollen (Flos Camelliae Japonicae) 0-10%, the smart powder 0-10% of Ganoderma herb, queen bee embryo dry powder 10%, Lac regis apis dry powder 5%.
---what the invention provides that described method makes is the auxiliary health-care effect health product that suppress tumor of having of raw material manufacturing with purification deleading propolis powder, and described health product are strong honeybee curing capsule, the deleading propolis powder 50% of wherein purifying, Ganoderma spore powder 50%.
---what the invention provides that described method makes is having blood lipid regulation and improving gastrointestinal function, facilitating digestion, loosening bowel to relieve constipation, gastric mucosa is had the health-care effect health product of auxiliary protection function of raw material manufacturing with purification deleading propolis powder; described health product are bee glue powder capsule; the deleading propolis powder 75-100% that wherein purifies, cyclodextrin 0-25% or polyvinylpyrrolidone 0-25% or superfine SiO 2 0-25%.
---the invention provides that described method makes with purification deleading propolis powder be the raw material manufacturing have cleaning throat and moistening larynx and radiation-resistant health-care effect health product, described health product are propolis dripping pill, the deleading propolis powder 10-50% that wherein purifies, Polyethylene glycol or polyoxyethylene (40) monostearate 50-90%.
---what the invention provides that described method makes is having prevention and treating the health product of each phase gastritis, gastric ulcer and duodenal ulcer, diabetes, cardiovascular and cerebrovascular disease, heart disease, hyperlipidemia, hypertension, coronary heart disease, psoriasis and viral hepatitis and influenza of raw material manufacturing with purification deleading propolis powder, described health product are bee glue powder capsule, the deleading propolis powder 75-100% that wherein purifies, cyclodextrin 0-25% or polyvinylpyrrolidone 0-25% or superfine SiO 2 0-25%.
---what the invention provides that described method makes is having prevention and treating the health product of each phase gastritis, gastric ulcer and duodenal ulcer, diabetes, cardiovascular and cerebrovascular disease, heart disease, hyperlipidemia, hypertension, coronary heart disease, psoriasis and viral hepatitis and influenza of raw material manufacturing with purification deleading propolis powder, described health product are propolis tablet, the deleading propolis powder 50-100% that wherein purifies, other adjuvant 0-50%.
---what the invention provides that described method makes is having prevention and treating the health product of each phase gastritis, gastric ulcer and duodenal ulcer, diabetes, cardiovascular and cerebrovascular disease, heart disease, hyperlipidemia, hypertension, coronary heart disease, psoriasis and viral hepatitis and influenza of raw material manufacturing with purification deleading propolis powder, described health product are propolis dripping pill, the deleading propolis powder 10-50% that wherein purifies, Polyethylene glycol or polyoxyethylene (40) monostearate 50-90%.
---what the invention provides that described method makes is the health product that raw material is made with purification deleading propolis powder, described health product are full component solubility propolis liquid goods and propolis liquid goods, the content range of deleading propolis powder of wherein purifying is 10-50%, the content range of solvent is 50-90%, and solvent is respectively 95% edible ethanol, ethanol, glycerol, polyglycereol, propylene glycol (Propylene glycol), polypropylene glycol (Polypropylene glycol) and Polyethylene Glycol (Polyethylene glycol) or its compositions.
---what the invention provides that described method makes is the health product that raw material is made with purification deleading propolis powder, described health product are full component solubility propolis liquid and goods thereof, dosage forms such as concentrated solution for example for oral administration, oral cavity aerosol, spray, drop and soft capsule.
---what the invention provides that described method makes is the health product that raw material is made with purification deleading propolis powder, described health product are full component solubility propolis liquid goods, propolis liquid food for example, as: 1. Beijing propolis liquid, the deleading propolis powder 5-50% that wherein purifies, 95% edible ethanol or/and propylene glycol (Propylene glycol) or/and Polyethylene Glycol (Polyethylene glycol) or its compositions 50-95%; 2. propolis vigor soft capsule, the deleading propolis powder 10-50% that wherein purifies, 95% edible ethanol or/and propylene glycol (Propylene glycol) or/and Polyethylene Glycol (Polyethylene glycol) or its compositions 50-90%.
---the invention provides that described method makes with purification deleading propolis powder be the raw material manufacturing have radioprotective and blood sugar regulation health product, described health product are the healthy goods of full component solubility propolis liquid, its purification deleading propolis powder 5-50%, 95% edible ethanol or/and propylene glycol (Propylene glycol) or/and Polyethylene Glycol (Polyethyleneglycol) or its compositions 50-95%.
---what the invention provides that described method makes is having cleaning throat and moistening larynx and beauty treatment, the acne of dispelling, functions of removing chloasma, improving the health product of skin moisture and oil content health-care effect of raw material manufacturing with purification deleading propolis powder, described health product are full component solubility propolis liquid or propolis vigor soft capsule, the deleading propolis powder 10-50% that wherein purifies, Polyethylene Glycol (Polyethylene glycol) 50-90%.
---what the invention provides that described method makes is having prevention and treating the health product of the effect of each phase gastritis, gastric ulcer and duodenal ulcer, diabetes, cardiovascular and cerebrovascular disease, heart disease, hyperlipidemia, hypertension, coronary heart disease, psoriasis and viral hepatitis and influenza of raw material manufacturing with purification deleading propolis powder, described health product are full component solubility propolis liquid or its propolis vigor soft capsule, the deleading propolis powder 10-50% that wherein purifies, Polyethylene Glycol (Polyethylene glycol) 50-90%.
---what the invention provides that described method makes is the health product that raw material is made with purification deleading propolis powder, described health product are full component solubility external propolis liquid, the content range of deleading propolis powder of wherein purifying is 5-20%, the content range of solvent is 80-95%, solvent be respectively ethanol, propylene glycol (Propylene glycol), polypropylene glycol (Polypropylene glycol), Polyethylene Glycol (Polyethylene glycol) but, the transdermal of externals such as isopropyl alcohol, dimethyl sulfoxide, glycerol and glyceric acid fat promotes lyosoption.
---what the invention provides that described method makes is the health product that raw material is made with purification deleading propolis powder, and described health product are full component solubility propolis liquid and such as aerosol for external use, spray, eye drop, ear drop, baths, liniment and unguentum etc.
---what the invention provides that described method makes is the health product that raw material is made with purification deleading propolis powder, a kind of molecular clathrate of the deleading propolis powder of purifying, microcapsule, microsphere and nanoparticle etc. have targeting and have the instant propolis powder new formulation of slow-releasing and controlled-releasing action, it is characterized in that: the content range of purification deleading propolis powder is 10-50%, enclose, encapsulation, the content range of microsphere and nanoparticle carrier material is 50-90%, enclose, encapsulation, microsphere and nanoparticle carrier material are respectively: 1. carbamide (urea, carbonyl diamine), thiourea, deoxycholic acid and cyclodextrin and derivant thereof etc.; 2. gelatin, polyvinylpyrrolidone, polyacrylic acid, hydroxy methocel and hydroxyethyl-cellulose etc.; 3. ethyl cellulose, gelatin, arabic gum, polylactic acid, methyl acrylate copolymer, methacrylic acid copolymer, polyamide, polyvidone and VPVAC etc.; 4. gelatin, methyl methacrylate, methyl 2-cyanoacrylate, cyanacrylate, Tisuacryl, isobutylcyanoacrylate and methylmethacrylate etc.
---what the invention provides that described method makes is the health product that raw material is made with purification deleading propolis powder, and propolis flavone content reaches more than 90% in the described health product, and wherein pinaster element, chrysin and three kinds of flavone sums of galangin reach more than 72%.Described health product are the new formulations such as molecular clathrate, microcapsule, microsphere and nanoparticle of confection, chewing gum, chewing gum, tablet (comprising buccal tablet and effervescent tablet), oral cavity aerosol, spray, capsule, granule, instant, beverage, soft gelatin capsule and drop pill and propolis flavone.The production of described health product propolis flavone and preparation method adopt: macroporous resin adsorption eluting preparation method, column chromatography and supercritical fluid extraction preparation method etc.
Specifically realize as follows:
1. the molecular clathrate of propolis antivirus antioxidizing active extract and microcapsule formulation
1. the molecular clathrate preparation of propolis antivirus antioxidizing active extract, be meant propolis vigor element with molecular forms by enclose or be embedded in the molecule tubular structure of novel enclose material (as beta-schardinger dextrin-etc.) formed ultra micron to disperse thing be molecular clathrate (Inclusion Compound), claim molecular microcapsule again.Its molecule stereo structure is cylindrical shape in the form of a ring, and outside diameter of cylinder is about the 1.3-1.4 nanometer, and internal diameter is about the 0.7-0.8 nanometer, and the high 0.7-0.8 nanometer that is about of tube is a kind of nanoscale molecular microcapsule.
2. preparation technology: fully stir and oven dry pulverizing-propolis vigor element clathrate solid material powder-dissolving and filtration-propolis vigor element inclusion complex in solution-spray drying-instant powder of propolis clathrate after the plain pure powder of propolis vigor-with the dissolution with solvents of 2 times of amounts and filtrations-lysate adds excipient.
3. the characteristics of molecular clathrate new formulation: the molecular clathrate of propolis antivirus antioxidizing active extract can make propolis vigor element change to the permeability of film with combination of proteins, thereby increased the absorption of propolis vigor element, improved the bioavailability of propolis vigor element, reduce the using dosage of propolis vigor element, improved the mouthfeel of propolis vigor element.
2. the microsphere of propolis antivirus antioxidizing active extract and nanoparticle preparation
Nanoparticle (Nanocapsules) is a nanocapsule, is a kind of directed delivery system that has, its similar microcapsule, and dispersion is than microcapsule micronize more, the molecular association complex of likeness in form colloidal ion.The nanoparticle preparation of propolis antivirus antioxidizing active extract is exactly the nanoparticle of the encapsulation propolis vigor element made with natural high molecular substance such as gelatin, albumin and cellulose family etc., and diameter is about the 50-500 nanometer.
The invention solves the technical barrier in five these fields of taking off such as removing heavy metal lead and desensitization, and make its technical specification reach the top standard.For example, wherein: 1. heavy metal lead≤0.01ppm, hydrargyrum≤0.01ppm, arsenic≤0.01ppm; 2. removed main sensitization source, through Cavia porcellus anaphylaxis contrast experiment, its result is: positive before the desensitization, the desensitization back is negative; 3. Cera Flava and insoluble impurities are 0 to be that propolis active substance content is 100%; 4. organochlorine pesticide is residual does not detect; 5. the nonactive composition of soluble resin class is 0.Provide standardized purification deleading propolis powder raw materials for production for producing and make new formulations such as serial propolis food, the healthy goods of propolis and propolis medicine.
Compared with prior art, the present invention has following distinguishing feature and good effect:
1) the propolis antivirus antioxidizing active extract deleading propolis powder purity height of promptly purifying reaches 100%.
2) can not add any antiadhesives and the excipient bonding of can not luming under 40 ℃ of hot conditionss, and present the mobile fabulous powder body of foresythia, its solubility solid content is up to 99.9%;
3) demarcated antivirus antioxidizing active material---propolis total flavones and caffeinic content in the standard China propolis extract with high performance liquid chromatography first.Total flavone content in propolis has reached 10%, wherein pinocembrin (Pinocembrin), galangin (Galangin) and chrysin (Chrysin) sum 〉=8%; And the content of caffeic acid (Caffeic acid) is 1-1.5%;
4) bee glue purifying of Sheng Chaning has: purified Cera Flava and insoluble impurities, removed organochlorine pesticide residual, desensitize, removed heavy metal (plumbous and hydrargyrum arsenic etc.) and pollute and removed the nonactive composition of some soluble resin classes etc. five and take off new feature, wherein propolis removing heavy-metal (lead and hydrargyrum arsenic etc.) technology and desensitization technology are in the leading level in the world;
5) a series of production technologies and manufacturing process thereof involved in the present invention not only are adapted to Chinese propolis, and are adapted to the raw material propolis that the propolis production countries and regions in the worldwide such as Brazilian propolis, Japanese propolis, Korea S's propolis, Canadian propolis, New Zealand's propolis, U.S.'s propolis, Russian propolis, India's propolis, Korea's propolis and Taiwan propolis are produced;
6) solved full component water-soluble bee glue liquid production technology;
7) on the basis of full component water-soluble bee glue liquid production technology, innovated propolis soft capsule production technology, and propolis antivirus antioxidizing active thing is existed with molecularity, content can reach 50%.
8) new formulation production technologies such as the instant propolis powder of molecular clathrate, microcapsule, microsphere and nanoparticle have been innovated.
9) promptly purify deleading propolis powder and preparation thereof of the propolis antivirus antioxidizing active extract that utilizes the technology of the present invention to produce, its advantage has greatly improved the antibacterial preservation antioxidation activity and the anti-virus ability of bee glue product, make nearly thousand kinds of effective active components in the propolis keep getting off intactly, the fresh and alive food that makes the higher fatty acid high protein that is applicable in the preservation antioxidation is (as fruit, fresh meat, fish, shrimp) and beverage (fresh milk, fruit juice, fruit juice, kernel protein beverage etc.), extend to more than 2 years even the longer time by storing 2-8 hour originally with regard to going bad.
Below by instantiation the present invention is done further narration, but this is not to be concrete qualification to the scope of the invention.
Specific embodiments
Promptly the purify manufacturing example of deleading propolis powder of embodiment one, propolis antivirus antioxidizing active extract
1. with the raw material propolis of 200 kilograms of weight pre-freeze 24 hours under the condition below 0 ℃;
2. the raw material propolis after the pre-freeze is crushed to 40 purpose powder rapidly with common beater grinder;
3. 200 kg feed material propolis powder are joined lentamente in the propolis extraction pot that 800 kilogram of 95% edible ethanol is housed that is stirring then;
4. stir and extract after 12 hours, quiet to precipitating 12 hours, wherein mixing speed is 8 rev/mins, and the extraction temperature is a normal temperature laboratory;
5. adopting the aperture is that the micropore fine filtration technology of 100 nanometers is made with extra care filtration to supernatant;
6. remove heavy metal (lead and hydrargyrum arsenic etc.): adopt ion exchange resin that heavy metal (lead and hydrargyrum arsenic etc.) is carried out selectivity ion exchange and remove;
7. reclaim under reduced pressure ethanol and concentrate drying cool off placement back crushing screening and promptly get 80 kilograms of purification deleading propolis powder.
After measured: the propolis antivirus antioxidizing active extract promptly purify the deleading propolis powder 1. purity be 100%; 2. solid content is 99.9%; 3. heavy metal lead≤0.0lppm; 4. the content of propolis total flavones 〉=10%, three kinds of important antivirus antioxidizing effective active components wherein: pinocembrin (5,7-dihydroxy flavanone Pinocembrin), chrysin (5,7-dihydroxyflavone Chrysin) and galangin (3,5,7-trihydroxyflavone alcohol Galangin) sum 〉=8%, other propolis flavone such as rutin (Rutin), myricetin (Myricetin), Quercetin (Quercetin), the luxuriant and rich with fragrance alcohol of camphane (Kaempferol), apigenin (Apigenin), morin (Motin) and isorhamnetin (Isorhamnetin) equal size sum are 2%, the content of caffeic acid (Caffeicacid) is 1.1%, and propolis flavone and caffeinic detection method all adopt high performance liquid chromatography (HPLC).
The technical matters embodiment is taken off in embodiment two, propolis antivirus antioxidizing active extract purification five
1. purify Cera Flava and insoluble impurities:
1. with the raw material propolis of double centner weight pre-freeze 24 hours under the condition below 0 ℃;
2. the raw material propolis after the pre-freeze is crushed to 40 purpose powder rapidly with common beater grinder;
3. double centner raw material propolis powder is joined lentamente in the propolis extraction pot that 400 kilogram of 95% edible ethanol is housed that is stirring then;
4. stir and extract after 12 hours, quiet to precipitating 12 hours, wherein mixing speed is 10 rev/mins, and the extraction temperature is a normal temperature laboratory;
5. quiet to after the propolis supernatant be that the micropore fine filtration technology of 100 nanometers is made with extra care filtration finally with the aperture.
2. it is residual to remove organochlorine pesticide:
6. adopt adsorbent resin that chlorinated organics is had a selective absorption to carry out selective absorption and remove to organochlorine pesticide is residual;
3. remove the nonactive composition of resinae of some solubilities:
7. extract at room temperature is with the nonactive composition of resinae of the solubility of removing the hot ethanol stripping, is that the micropore fine filtration technology of 100 nanometers is made with extra care filtration with the aperture finally;
4. desensitization:
8. on the basis of the nonactive composition of resinae that purifies insoluble impurities and some solubilities, adopt adsorbent such as activated earth that sensitizer is carried out adsorbing and removing again, be that the micropore fine filtration technology of 100 nanometers is made with extra care filtration finally with the aperture.
5. remove heavy metal (lead and hydrargyrum arsenic etc.):
9. adopting ion exchange resin that heavy metal (plumbous and hydrargyrum arsenic etc.) is carried out selectivity ion exchange and remove, is that the micropore fine filtration technology of 100 nanometers is made with extra care filtration with the aperture finally.
6. reclaim under reduced pressure ethanol and concentrate drying:
10. reclaim under reduced pressure ethanol and concentrate drying cool off placement back crushing screening and promptly get 40 kilograms of propolis vigor elements.After measured, the propolis antivirus antioxidizing active extract is that the technical specification of propolis vigor element is:
1. Cera Flava and insoluble impurities are 0 to be that propolis active substance content is 100%;
2. organochlorine pesticide is residual does not detect;
3. the nonactive composition of soluble resin class is 0;
4. through Cavia porcellus anaphylaxis contrast experiment, its result is: positive before the desensitization, the desensitization back is negative;
5. heavy metal lead≤0.01ppm, hydrargyrum≤0.01ppm, arsenic≤0.01ppm.
Embodiment three, be the propolis food embodiment that main material production is made with purification deleading propolis powder
1. selenium spirit propolis powder (capsule): purification deleading propolis powder 20%, Ganoderma spore powder with cellular wall broken 20%, selenium-enriched edible mushroom powder 20%, cyclodextrin 40%.
2. propolis powder (capsule): purification deleading propolis powder 85%, cyclodextrin 15%.
3. propolis ganoderma lucidum outstanding person (capsule): 50 parts of weight of Ganoderma spore powder with cellular wall broken, 25 parts of weight of purification deleading propolis powder, 25 parts of weight of cyclodextrin, 20 parts of weight of queen bee embryo dry powder.
4. the compound extraordinary bee pollen of propolis (electuary): purification deleading propolis powder 10%, bee pollen 90%.
Example four, be the healthy goods example I of propolis that main material production is made with purification deleading propolis powder
1. has the healthy goods of propolis that improve sleep and chemical liver injury is had auxiliary protection function---selenium spirit propolis powder (capsule).It consists of: purification deleading propolis powder 20-50%, Ganoderma spore powder with cellular wall broken 20-25%, selenium-enriched edible mushroom powder (health must selenium powder) 20-25%, cyclodextrin 0-40%.
2. has healthy goods---the propolis powder (capsule) of the propolis that improves gastrointestinal function (facilitating digestion/loosening bowel to relieve constipation/gastric mucosa is had auxiliary protection function).It consists of: purification deleading propolis powder 75-100%, superfine SiO 2 0-25%.
3. the propolis healthy goods---honeybee Lingbao City (capsule) that has auxiliary function of tumor inhibition.It consists of: Ganoderma spore powder with cellular wall broken 50%, purification deleading propolis powder 25%, broker wall bee pollen (Flos Camelliae Japonicae) 0-10%, the smart powder 0-10% of Ganoderma herb, queen bee embryo dry powder 10%, Lac regis apis dry powder 5%.
4. the healthy goods of propolis---the strong honeybee spirit (capsule) that has auxiliary function of tumor inhibition.It consists of: purification deleading propolis powder 50%, Ganoderma spore powder 50%.
Example five, be the healthy goods example II of propolis that main material production is made with purification deleading propolis powder
1. has healthy goods---the propolis powder (capsule) of the propolis that prevents and treat each phase gastritis, gastric ulcer and duodenal ulcer, diabetes, cardiovascular and cerebrovascular disease, heart disease, hyperlipidemia, hypertension, coronary heart disease, psoriasis and viral hepatitis and influenza effect.It consists of: purification deleading propolis powder 75-100%, cyclodextrin 0-25%.
2. has healthy goods---the propolis tablet (tablet) of the propolis that prevents and treat each phase gastritis, gastric ulcer and duodenal ulcer, diabetes, cardiovascular and cerebrovascular disease, heart disease, hyperlipidemia, hypertension, coronary heart disease, psoriasis and viral hepatitis and influenza effect.It consists of: purification deleading propolis powder 50-100%, other adjuvant 0-50%.
3. has healthy goods---the propolis dripping pill of the propolis that prevents and treat each phase gastritis, gastric ulcer and duodenal ulcer, diabetes, cardiovascular and cerebrovascular disease, heart disease, hyperlipidemia, hypertension, coronary heart disease, psoriasis and viral hepatitis and influenza effect.It consists of: purification deleading propolis powder 10-50%, Polyethylene glycol or polyoxyethylene (40) monostearate (S-40) 50-90%.
Example six, be the propolis food embodiment that main material production is made with full component solubility propolis liquid
1. in the propolis liquid of Beijing: purification deleading propolis powder 10-50%, Propylene glycol is or/and Polyethyleneglycol or its compositions 50-90%.
2. in the propolis vigor soft capsule: purification deleading propolis powder 10-50%, Polyethylene glycol 50-90%.
Example seven, be the propolis health food embodiment that raw material production is made with full component solubility propolis liquid
1. have in Beijing propolis liquid of health cares such as immunomodulating and blood sugar regulation: purification deleading propolis powder 10-50%, Propylene glycol is or/and Polyethylene glycol or its compositions 50-90%.
2. have in the propolis vigor soft capsule of health cares such as blood sugar regulation and beauty treatment (acne/functions of removing chloasma of dispelling/improve skin moisture and oil content): purification deleading propolis powder 10-50%, Polyethylene glycol50-90%.
3. have in the propolis dripping pill of health cares such as cleaning throat and moistening larynx and radioprotective: purification deleading propolis powder 10-50%, Polyethylene glycol 50-90%.
Example eight, be the bee glue product example I that raw material production is made with full component solubility propolis liquid
With full component solubility propolis liquid is bee glue product-rheumatism essence that main material production is made, and its manufacture method is as follows:
1. the fresh Venenum apis of 0.5-1% is added in the full component solubility of the 5-20% propolis liquid, and then add an amount of Mentholum, essential oil and eugenol etc., fully mix the back packing and promptly get the rheumatism essence.
2. the rheumatism essence is a kind of externally applied liniment, is mainly used in rheumatism, rheumatoid arthrosis osteodynia, mosquito bite.
Example nine, be the healthy goods example II of propolis that raw material production is made with full component solubility propolis liquid
1. have the prevention and treat in the propolis vigor soft capsule of each phase gastritis, gastric ulcer and duodenal ulcer, diabetes, cardiovascular and cerebrovascular disease, heart disease, hyperlipidemia, hypertension, coronary heart disease, psoriasis and viral hepatitis and influenza effect: purification deleading propolis powder 10-50%, Polyethylene glycol 50-90%.
2. have the prevention and treat in the propolis dripping pill of each phase gastritis, gastric ulcer and duodenal ulcer, diabetes, cardiovascular and cerebrovascular disease, heart disease, hyperlipidemia, hypertension, coronary heart disease, psoriasis and viral hepatitis and influenza effect: purification deleading propolis powder 10-50%, Polyethylene glycol 50-90%.
Example ten, be primary raw material with purification deleading propolis powder, with supercritical liquid extraction technique production and preparation propolis flavone embodiment
1. supercritical extraction technique is the efficient abstraction technique that development in recent years is got up, and it is to utilize the property of medium under supercriticality, under different pressure and temperatures, can optionally extract the active substance composition in the raw material.
2. the present invention adopts the supercritical fluid extraction machine, with CO 2Make medium the propolis flavone in the purification deleading propolis has been carried out optionally extraction.
3. propolis flavone supercritical extraction liquid is through concentrate under reduced pressure at low temperature, and promptly gets propolis flavone after the drying and crushing.After measured: propolis flavone content 95%, wherein pinaster element, chrysin and galangin sum are 76%, detection method adopts high performance liquid chromatography (HPLC).
Example 11, be main material production and make propolis flavone goods example I with the supercritical propolis flavone
With the supercritical propolis flavone is main material production propolis flavone drop pill, and its manufacture method is as follows:
1. after using Polyethylene glycol with the fusion of supercritical propolis flavone, directly drip system propolis flavone drop pill.
2. in the propolis flavone drop pill: supercritical propolis flavone 50%, Polyethylene glycol 50%.
After measured: in the propolis flavone drop pill---propolis flavone content 47.5%, wherein pinaster element, chrysin and galangin sum are 38%, detection method adopts high performance liquid chromatography (HPLC).
Example 12, be main material production and make propolis flavone goods example II with the supercritical propolis flavone
With the supercritical propolis flavone is the instant powder of main material production propolis flavone, and its manufacture method is as follows:
1. with the supercritical propolis flavone with organic solvent dissolution after, directly add in the saturated solution of cyclodextrin, and constantly stir, the cooling post crystallization promptly gets the instant powder of propolis flavone.
2. in the instant powder of propolis flavone: supercritical propolis flavone 10%, cyclodextrin 90%.
After measured: in the instant powder of propolis flavone---propolis flavone content 9.5%, wherein pinaster element, chrysin and galangin sum are 7.6%, detection method adopts high performance liquid chromatography (HPLC).

Claims (1)

1. method for preparing the deleading propolis is characterized in that this method comprises:
1, with the raw material propolis more than-4 ℃ to 0 ℃ the temperature pre-freeze,
2, after the pre-freeze, be crushed to below 40 orders,
3, room temperature and under 8-15 rev/min of mixing speed, with ethanol extraction 8-12 hour that equals greater than 95% percetage by weight, propolis powder was 1 than 3.5-4.5 with equaling weight ratio greater than the ethanol extraction solvent of 95% percetage by weight,
4, filter with micropore fine filtration technology,
5, after the secondary filter, use the resin that chlorinated organics is had a selective absorption to remove,
6, carry out the adsorbing and removing sensitizer with the activated earth adsorbent,
7, use the ion exchange resin that heavy metal is had a selective absorption to carry out selective absorption, remove heavy metal,
8, extract at room temperature is with the resinae non-active ingredient of the solubility of removing the hot ethanol stripping,
9, be that the micropore fine filtration technology of 100 nanometers is made with extra care filtration with the aperture,
10, the propolis powder that drying under reduced pressure is pulverized.
CNB011417633A 2001-09-18 2001-09-18 Antivirus antioxidizing active extract of proplis and its molecular inclusion compound Expired - Fee Related CN1220497C (en)

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