CN101991606A - Preparation method of solid water-soluble lead-removed propolis - Google Patents
Preparation method of solid water-soluble lead-removed propolis Download PDFInfo
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- CN101991606A CN101991606A CN200910065753XA CN200910065753A CN101991606A CN 101991606 A CN101991606 A CN 101991606A CN 200910065753X A CN200910065753X A CN 200910065753XA CN 200910065753 A CN200910065753 A CN 200910065753A CN 101991606 A CN101991606 A CN 101991606A
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Abstract
The invention relates to a preparation method of solid water-soluble lead-removed propolis, which belongs to the field of deep processing technology of proplis. The propolis is mainly prepared by the following steps of: adding 50 to 90 percent ethanol into 10 to 50 weight parts of propolis raw powder; stirring at normal temperature and leaching for 6 to 24 hours; lowering the temperature to 0 to 8 DEG C with circulating cold saline and performing cold leaching for 2 to 12 hours; centrifugally filtering at the speed of between 1,000 and 6,000 rpm; performing chromatography on filtrate by using an acid cation exchange resin chromatographic column; decompressing chromatographic solution and removing the ethanol so as to obtain concentrated solution with the relative density of 1.28; dissolving the concentrated solution in purified aqueous solution which contains 5 to 50 percent of starch glycolipid; emulsifying by using a homogenizer or a colloid mill; and performing spray drying or vacuum decompression drying on emulsified liquid so as to obtain the solid water-soluble propolis. Detection on the propolis produced by the preparation method indicates that the total flavonoid content of the propolis is more than or equal to 13.86 mg/g and the lead content is less than or equal to 0.03 ppm, wherein the total flavonoid serves as a marking component.
Description
Technical field
The present invention relates to a kind of propolis deep process field, be specifically related to a kind of preparation method of solid, water soluble deleading propolis.
Background technology
Propolis belongs to all-natural product as a kind of mixture of animals and plants secretions, have no side effect, and proof has good safety and extensive, stable preventing and curing diseases and health-care effect after deliberation, has caused countries in the world scientists' great attention.Research and clinical confirmation both at home and abroad, propolis has infection, antiviral, antitumor, antioxidation, resisting fatigue, radioprotective; Blood fat reducing, blood sugar lowering, blood pressure lowering, cholesterol reducing; Enhance immunity, removing free radical, beauty treatment, promotion tissue regeneration effect.Wherein, the most significant effect is that antibacterial, fungus, virus are all had inhibition, killing action, is a kind of natural wide spectrum antibiotics of preciousness.By the scientists laudatory title " the most perfect natural antibiotics ", " natural immunity reinforcing agent ", " blood vessel street cleaner ", " Natural antioxidant " etc.2002, propolis was formally listed in " the article list that can be used for health food " by Ministry of Public Health, was formally listed in the Pharmacopoeia of the People's Republic of China, and became legal simply Chinese medicine in 2005.
Natural propolis is a kind of resinae material of complicated component, comprises flavone compound; Phenol, aldehyde, ketone, ester, ether compound; Alcohol compound; Alkene, hydrocarbon, compounds; Trace element and other chemical compounds such as polysaccharide and vitamin etc. are its bases with extensive physiologically active and health-care effect.Natural propolis can not directly eat owing to containing harmful heavy metals such as many non-effect impurity and lead, must extract purification to it and just can be used for prevention and health care.But the dissolubility of propolis in water is very little, is dissolved in solution such as ethanol, alkali, acetone, and traditional extracting method is to adopt ethanol extraction, is difficult to bring into play the maximum effect of propolis, can not effectively remove heavy metals such as lead.Through scientist's continuous effort, the processing technique of propolis has had bigger progress.As: CN1162613A, CN1360897A have announced that different concentration ethanol dissolves, leaves standstill, filters, cools off the technology of extracting propolis to propolis, handle but heavy metals such as lead are done to remove.CN1277816A announced with liquid nitrogen cryogenics pulverize, ethanol merceration, the critical freezing sedimentation technology of getting rid of filtering lead, vacuum and low temperature concentrating under reduced pressure repeatedly, CN1868312A has announced with airtight multiple extraction, the high speed centrifugation deleading of alcohol at normal temperature, the exsiccant technology of vacuum concentration, CN101061834A has announced with pulverize at low temperature, dissolve with ethanol, ultrasonic extraction, has left standstill, resin column absorption deleading, vacuum concentration, Quercus acutissima Carr. storage tank are brewageed the technology of ripening, though above technology has been carried out the deleading processing in extraction, do not consider the water solublity of propolis.CN1462512A has announced with ethanol and has slightly carried and deleading, the technology that adds 80 ℃ of preparations of Polyethylene Glycol heating water-soluble bee glue liquid, CN1108057A has announced with glycerol and has soaked, heating, stir, filter the technology of preparation water-soluble bee glue liquid, CN1644086A has announced with caustic soda solution heating for dissolving propolis, add Chinese medicine ingredients, continue heating, vacuum is flung to the technology that moisture prepares solid water soluble propolis, and CN1839890A has announced with water and soaked the extraction propolis earlier, tell solids petroleum ether reflux, extract,, extracting solution reuse ethanol and acetone mixed-liquor return extract, distillation is dry, dry thing adds in L-arginine or the L-lysine solution, separate out solids, the solution lyophilization.
Above technology or use organic solvent or and use highly basic or and use high temperature or use above-mentioned condition simultaneously, make the propolis of being produced or be alcoholic solution, make and should not use the ethanol allergy sufferers; The use organic solvent is removed and is not caused secondary pollution only; Use technologies such as highly basic or high temperature, make effective bee glue components lost; Only look after deleading and do not take into account water solublity, or only look after water solublity and do not take into account deleading, limited the application of propolis and the performance of medicinal health care function undoubtedly in some aspects.
Natural propolis contains have an appointment 55% resin and balsam, 30% Cera Flava, 10% fragrant volatile oil, 5% foreign material such as pollen.Its chemical constituent comprises flavone compound, acid, alcohol, phenol, aldehyde, ester, ether and alkene, terpenoid and several amino acids, fatty acid, enzyme, vitamin, trace element etc., have good safety and extensive, stable preventing and curing diseases and health-care effect, in food, medicine, be widely used.China's industry standard regulation, the lead of the common product of propolis class (as propolis liquid, bee glue soft capsule etc.) must not limit the quantity of above 0.5mg/kg, and lead tolerance surpasses tens times of this standards in some propolis raw material, so the propolis of handling without strict deleading technique is that anorexia is used.Remove and control lead content in the propolis on the source, the propolis deleading technique is taked absorption method, chemical precipitation method, supercritical extraction etc. usually in processing link.Adopt adsorbents adsorb deleadings such as active carbon, its effect can not guarantee and adsorbent such as active carbon can adsorb a large amount of flavonoids effective constituents, thereby cause a large amount of losses of functional component, adopt technology deleadings such as the lixiviate of gradient ethanol, freezing sedimentation, supercritical extraction propolis etc., its deleading is respond well, but the equipment requirements height, complicated operation is not suitable for popular the popularization.
Summary of the invention
The objective of the invention is to overcome above-mentioned deficiency, the preparation method of the solid, water soluble deleading propolis that a kind of effective bee glue components destroys less, extracts fully, low, the no organic solvent of content of heavy metal lead is residual, easy to use is provided.When farthest keeping the natural propolis active component, the content of propolis heavy metal lead is reduced greatly, use more convenient, use face is more extensive, really these health product from time immemorial have been brought into modern's life, for vast chronic disease and sub-health population provide a kind of safe, propolis product efficiently.
Technology contents of the present invention is: a kind of preparation method of solid, water soluble deleading propolis: 10～50 weight portion honeybee collagen powder are added 50%～90% alcohol at normal temperature stirring and leaching 6～24 hours, be cooled to 0～8 ℃ of merceration 2～12 hours with the circulation cool brine, get rid of filter through 1000～6000rpm is centrifugal, filtrate is through acid cation exchange resin chromatographic column chromatography, the chromatographic solution decompression removes ethanol, obtain relative density and be 1.28 concentrated solution, concentrated solution is dissolved in the purification of aqueous solutions that contains 5%～50% starch glycolipid, use homogenizer or colloid mill to carry out emulsifying, the spray-dried or dry preparation solid water soluble propolis of vacuum decompression of emulsion.
Preferred for preparation method of the present invention is: 20 weight portion honeybee collagen powder are added 75% alcohol at normal temperature stirring and leaching 12 hours, be cooled to 5 ℃ of mercerations 6 hours with the circulation cool brine, get rid of filter through 3000rpm is centrifugal, filtrate is through acid cation exchange resin chromatographic column chromatography, after removing ethanol, the chromatographic solution decompression dissolves in the purification of aqueous solutions that contains 25% starch glycolipid, carry out emulsifying with homogenizer or colloid mill, the spray-dried microcapsule propolis powder that gets of emulsion.
The pH of the chromatographic column of described acid cation exchange resin is 3～7, with the nitric acid of 3mol/L saturated resin is carried out eluting regeneration.
Described starch glycolipid is a kind of in succinic acid (acid anhydride) the starch glycolipid of octenyl, capric acid base, dodecenyl succinic, tetradecene base, hexadecene base, vaccenic acid base, or their mixture.
Beneficial effect of the present invention is:
1. effective bee glue components extraction ratio height, low, the no organic solvent of content of heavy metal lead are residual.Reduce the propolis of production after testing with the present invention, the significant composition general flavone content 〉=13.86mg/g of propolis, lead content≤0.03ppm.
2. finished product is the dark brown powder, has the peculiar fragrant of natural propolis.Soluble in water, it is fast to take post-absorption, and the bioavailability height helps the performance of propolis medical health care function.
3. used starch sugar ester is novel food emulsifying agent, and WHO/FAO (INS:1450 nineteen eighty-two) is evaluated as safe novel food emulsifying agent, and a day permission intake need not to do special regulation, and to this kind of starch scope of application without limits.Ratified this product in 1997 in China and use on food as food additive, calendar year 2001 has ratified to enlarge the scope that this product uses again in food, and consumption can add according to demand, need not control.
4. water-soluble powder is convenient to be processed into different dosage forms, and water-soluble powder can satisfy different consumer groups' different demands for the production of follow-up finished product provides multiple dosage form selection.As can be made into capsule, granule, buccal tablet or chew health food, the medical supplies of tablet, soft capsule, oral liquid and other solutions such as sheet.
The specific embodiment
Below by embodiment the present invention is elaborated, but and do not limit the present invention in any way.
Embodiment 1
(1) preparation of solid, water soluble deleading propolis
20 weight portion honeybee collagen powder are placed the interlayer extraction pot of band stirring, add 75% ethanol water stirring at normal temperature lixiviate 12 hours, be cooled to 5 ℃ of mercerations 6 hours with the circulation cool brine, the merceration thing is put into the centrifuge that 100 order nylon filter clothes are housed, get rid of filter through 3000rpm is centrifugal, filtrate is through acid cation exchange resin chromatographic column chromatography, the chromatographic solution decompression removes ethanol, obtain relative density and be 1.28 concentrated solution, concentrated solution is dissolved in the purification of aqueous solutions that contains 25% starch octenyl succinate anhydride, carried out the emulsifying homogenizing 30 minutes with homogenizer, emulsion is spray-dried, promptly gets solid, water soluble deleading propolis.
(2) the capsular preparation of water-soluble lead-off propolis
Water-soluble lead-off propolis 50 weight portions, soluble starch 30 weight portions, mix homogeneously is measured filling on demand in hard capsule, polishing, packing.
Embodiment 2
(1) preparation of solid, water soluble deleading propolis
30 weight portion honeybee collagen powder are placed the interlayer extraction pot of band stirring, add 80% ethanol water stirring at normal temperature lixiviate 16 hours, be cooled to 5 ℃ of mercerations 8 hours with the circulation cool brine, the merceration thing is put into the centrifuge that 100 order nylon filter clothes are housed, get rid of filter through 4000rpm is centrifugal, filtrate is through acid cation exchange resin chromatographic column chromatography, the chromatographic solution decompression removes ethanol, obtain relative density and be 1.28 concentrated solution, concentrated solution is dissolved in the purification of aqueous solutions that contains 25% capric acid base succinic acid starch ester, carried out the emulsifying homogenizing 30 minutes with homogenizer, emulsion is spray-dried, promptly gets solid, water soluble deleading propolis.
(2) the particulate preparation of water-soluble lead-off propolis
Water-soluble lead-off propolis 80 weight portions, soluble starch 60 weight portions, 5% starch slurry, 8 weight portions, mixing granulation, the essence of 0.6 weight portion is put and is sprayed in 60 ℃ of oven dry of wet granular in order, on demand the amount packing.
Embodiment 3
(1) preparation of solid, water soluble deleading propolis
10 weight portion honeybee collagen powder are placed the interlayer extraction pot of band stirring, add 60% ethanol water stirring at normal temperature lixiviate 8 hours, be cooled to 5 ℃ of mercerations 5 hours with the circulation cool brine, the merceration thing is put into the centrifuge that 100 order nylon filter clothes are housed, get rid of filter through 2000rpm is centrifugal, filtrate is through acid cation exchange resin chromatographic column chromatography, the chromatographic solution decompression removes ethanol, obtain relative density and be 1.28 concentrated solution, concentrated solution is dissolved in the purification of aqueous solutions that contains 25% capric acid base succinic acid starch ester, carried out the emulsifying homogenizing 30 minutes with homogenizer, emulsion is spray-dried, promptly gets solid, water soluble deleading propolis.
(2) preparation of water-soluble lead-off propolis sheet
Water-soluble lead-off propolis 20 weight portions, amylum pregelatinisatum 40 weight portions, microcrystalline Cellulose 30 weight portions, magnesium stearate 2 weight portions, mix homogeneously, sheet weight sheet is packed on demand.
Embodiment 4
(1) preparation of solid, water soluble deleading propolis
40 weight portion honeybee collagen powder are placed the interlayer extraction pot of band stirring, add 90% ethanol water stirring at normal temperature lixiviate 14 hours, be cooled to 5 ℃ of mercerations 5 hours with the circulation cool brine, the merceration thing is put into the centrifuge that 100 order nylon filter clothes are housed, get rid of filter through 5000rpm is centrifugal, filtrate is through acid cation exchange resin chromatographic column chromatography, the chromatographic solution decompression removes ethanol, obtain relative density and be 1.28 concentrated solution, concentrated solution is dissolved in the purification of aqueous solutions that contains 40% dodecenyl succinic succinic acid starch ester, carried out the emulsifying homogenizing 30 minutes with homogenizer, emulsion is spray-dried, promptly gets solid, water soluble deleading propolis.
(2) preparation of water-soluble lead-off propolis buccal tablet (chewing sheet)
Water-soluble lead-off propolis 50 weight portions, glucose powder 60 weight portions, xylitol 20 weight portions, microcrystalline Cellulose 15 weight portions, Mentholum microcrystalline Cellulose 4 weight portions, Fructus Citri tangerinae essence 6 weight portions, magnesium stearate 3 weight portions, mix homogeneously, sheet weight sheet is packed on demand.
Embodiment 5
(1) preparation of solid, water soluble deleading propolis
30 weight portion honeybee collagen powder are placed the interlayer extraction pot of band stirring, add 70% ethanol water stirring at normal temperature lixiviate 16 hours, be cooled to 5 ℃ of mac per hor Xs with the circulation cool brine, the merceration thing is put into the centrifuge that 100 order nylon filter clothes are housed, get rid of filter through 3000rpm is centrifugal, filtrate is through acid cation exchange resin chromatographic column chromatography, the chromatographic solution decompression removes ethanol, obtain relative density and be 1.28 concentrated solution, concentrated solution is dissolved in the purification of aqueous solutions that contains 40% tetradecene base succinic acid starch ester, carried out the emulsifying homogenizing 30 minutes with homogenizer, emulsion is spray-dried, promptly gets solid, water soluble deleading propolis.
(2) water-soluble lead-off propolis preparation of soft capsule
Water-soluble lead-off propolis 50 weight portions, vegetable oil 30 weight portions, edible Gelatinum oxhide 40 weight portions, glycerol 20 weight portions are made soft capsule through colloidal sol, batching, pelleting, drying, packing.
Embodiment 6
(1) preparation of solid, water soluble deleading propolis
40 weight portion honeybee collagen powder are placed the interlayer extraction pot of band stirring, add 80% ethanol water stirring at normal temperature lixiviate 18 hours, be cooled to 5 ℃ of mac per hor Xs with the circulation cool brine, the merceration thing is put into the centrifuge that 100 order nylon filter clothes are housed, get rid of filter through 5000rpm is centrifugal, filtrate is through acid cation exchange resin chromatographic column chromatography, the chromatographic solution decompression removes ethanol, obtain relative density and be 1.28 concentrated solution, concentrated solution is dissolved in the purification of aqueous solutions that contains 40% vaccenic acid base succinic acid starch ester, carried out the emulsifying homogenizing 30 minutes with homogenizer, emulsion is spray-dried, promptly gets solid, water soluble deleading propolis.
(2) preparation of water-soluble lead-off propolis oral liquid
Water-soluble lead-off propolis 40 weight portions, stevioside's 6 weight portions, edible essence 2 weight portions, purified water 60 weight portions are made oral liquid through dissolving, mixing, fill, sterilization.
After understanding content of the present invention, various equivalent modifications such as honeybee finished product, medicine, health care, nutrition, food can be done this improvement or change to the present invention, and the change of these equivalent form of values falls within the application's appended claims institute restricted portion equally.
Claims (6)
1. the preparation method of a solid, water soluble deleading propolis, it is characterized in that it is undertaken by following step: 10～50 weight portion honeybee collagen powder are added 50%～90% alcohol at normal temperature stirring and leaching 6～24 hours, be cooled to 0～8 ℃ of merceration 2～12 hours with the circulation cool brine, get rid of filter through 1000～6000rpm is centrifugal, filtrate is through acid cation exchange resin chromatographic column chromatography, the chromatographic solution decompression is dissolved in the purification of aqueous solutions that contains 5%～50% starch glycolipid and emulsifying after removing ethanol, the spray-dried or dry preparation solid water soluble propolis of vacuum decompression of emulsion.
2. the preparation method of solid, water soluble deleading propolis according to claim 1, it is characterized in that: 20 weight portion honeybee collagen powder are added 75% alcohol at normal temperature stirring and leaching 12 hours, be cooled to 5 ℃ of mercerations 6 hours with the circulation cool brine, get rid of filter through 3000rpm is centrifugal, filtrate is through acid cation exchange resin chromatographic column chromatography, the chromatographic solution decompression is dissolved in the purification of aqueous solutions that contains 25% starch glycolipid and emulsifying after removing ethanol, the spray-dried microcapsule propolis powder that gets of emulsion.
3. the preparation method of solid, water soluble deleading propolis according to claim 1 and 2 is characterized in that: the pH of the chromatographic column of described acid cation exchange resin is 3～7, with the nitric acid of 3mol/L saturated resin is carried out eluting regeneration.
4. the preparation method of solid, water soluble deleading propolis according to claim 1 and 2, it is characterized in that: described starch glycolipid is a kind of in succinic acid (acid anhydride) the starch glycolipid of octenyl, capric acid base, dodecenyl succinic, tetradecene base, hexadecene base, vaccenic acid base, or their mixture.
5. the preparation method of solid, water soluble deleading propolis according to claim 1 and 2 is characterized in that: it is 1.28 that the chromatographic solution decompression recycling ethanol concentrates the back relative density.
6. the preparation method of solid, water soluble deleading propolis according to claim 1 and 2 is characterized in that: the emulsion process of described emulsion is used homogenizer or colloid mill.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110639226A (en) * | 2019-09-24 | 2020-01-03 | 江苏蜂奥生物科技有限公司 | Method for removing impurities in propolis |
| CN110665470A (en) * | 2019-09-24 | 2020-01-10 | 江苏蜂奥生物科技有限公司 | Adsorbent used in propolis extraction process and preparation method thereof |
| CN113750120A (en) * | 2021-10-11 | 2021-12-07 | 北京德蜂堂健康科技有限公司 | Propolis extract and production process and application thereof |
| CN113926218A (en) * | 2021-11-15 | 2022-01-14 | 老蜂农生物科技集团有限公司 | Production process of propolis ethanol extract and propolis ethanol extract |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4446502B2 (en) * | 1998-07-31 | 2010-04-07 | 株式会社林原生物化学研究所 | Propolis extract |
| JP2003219814A (en) * | 2002-01-30 | 2003-08-05 | Yokohama Yushi Kogyo Kk | Propolis composition easily dispersible in water |
| CN1283261C (en) * | 2003-06-08 | 2006-11-08 | 刘进祖 | Water-soluble propolis liquor and its preparation method |
| CN1313020C (en) * | 2003-12-25 | 2007-05-02 | 南昌大学 | Combination use of absorption and ion exchange for removing lead from propolis |
-
2009
- 2009-08-12 CN CN200910065753XA patent/CN101991606B/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110639226A (en) * | 2019-09-24 | 2020-01-03 | 江苏蜂奥生物科技有限公司 | Method for removing impurities in propolis |
| CN110665470A (en) * | 2019-09-24 | 2020-01-10 | 江苏蜂奥生物科技有限公司 | Adsorbent used in propolis extraction process and preparation method thereof |
| CN113750120A (en) * | 2021-10-11 | 2021-12-07 | 北京德蜂堂健康科技有限公司 | Propolis extract and production process and application thereof |
| CN113750120B (en) * | 2021-10-11 | 2023-10-24 | 北京德蜂堂健康科技有限公司 | Propolis extract and production process and application thereof |
| CN113926218A (en) * | 2021-11-15 | 2022-01-14 | 老蜂农生物科技集团有限公司 | Production process of propolis ethanol extract and propolis ethanol extract |
| CN113926218B (en) * | 2021-11-15 | 2022-12-06 | 老蜂农生物科技集团有限公司 | Production process of propolis ethanol extract and propolis ethanol extract |
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| CN101991606B (en) | 2012-07-04 |
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