CN107158046A - A kind of total ganoderma spore powder removes wall micropill - Google Patents

A kind of total ganoderma spore powder removes wall micropill Download PDF

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CN107158046A
CN107158046A CN201710511241.6A CN201710511241A CN107158046A CN 107158046 A CN107158046 A CN 107158046A CN 201710511241 A CN201710511241 A CN 201710511241A CN 107158046 A CN107158046 A CN 107158046A
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micropill
weight
spore powder
extract
wall
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CN107158046B (en
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李赛飞
晏礼明
文华安
陈彩霞
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Institute of Microbiology of CAS
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/06Fungi, e.g. yeasts
    • A61K36/07Basidiomycota, e.g. Cryptococcus
    • A61K36/074Ganoderma
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/48Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/50Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
    • A61K9/5005Wall or coating material
    • A61K9/5021Organic macromolecular compounds
    • A61K9/5036Polysaccharides, e.g. gums, alginate; Cyclodextrin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/37Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps

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Abstract

The present invention provides a kind of total ganoderma spore powder and removes wall micropill, and its active component is carbon dioxide abstraction thing, ethanol extract and the water extract comprising lucidum spore powder being embedded in micropill shell, and the part by weight of three is 34: 1: 34.The total ganoderma spore powder goes wall micropill to be prepared by following step:Viscosity after the liquid carbon dioxide extract, ethanol extract and water extract of lucidum spore powder are mixed with 0.5% 5 weight % mixes for 20 800cps sodium alginate aqueous solution, stir while in droplets, in the calcium chloride water for dripping to 0.5 5 weight %, form microspheric granula, after the microspheric granula formed soaks 1 240 minutes in 0.5 5 weight % calcium chloride water, take out, after being cleaned up in distilled water, dry, obtain total ganoderma spore powder and remove wall micropill.

Description

A kind of total ganoderma spore powder removes wall micropill
Technical field
Wall micropill and the method for preparing it are removed the present invention relates to a kind of total ganoderma spore powder, belongs to field of medicaments.
Background technology
Lucidum spore powder is the elite of ganoderma lucidum, containing abundant bioactive ingredients, with important medicinal health function.Spirit The main component that Ganoderma lucidum spore powder plays effect is a series of bioactive substances such as GL-B and ganodenic acid, these active matters Matter is wrapped in hard conidial cell wall, only by breaking trachytectum of glossy ganoderma, and active ingredient could discharge utilization.Carried according to modern times separation Take the active material of different qualities in technology, lucidum spore powder to need to extract by different Extraction solvents, such as pass through food Level liquid carbon dioxide Ganoderma Lucidum Spores Oil Extracted, can extract unrighted acid, ganodenic acid isoreactivity composition, ethanol Extraction the medium active material extraction of triterpenes and polarity can be gone out, hot water extraction then the polysaccharide of main extracting ganoderma, The materials such as polypeptide, amino acid.The class material of the above three represents the powerful material of institute that conidia powder is included substantially, and proportion is about For the 50-60% of conidia powder, remaining 40-50% is not available Reishi sporule wall.
There are following two broad aspects using aspect in current lucidum spore powder:
First, traditional lucidum spore powder is typically that direct packaging is into using after pouch or filling capsule after broken wall, and it is deposited Defect have:
1,1 part of conidia powder product is taken, its weight half is the conidial cell wall of without effect, and the active ingredient really absorbed only has Half, absorption rate is low;
2, conidia powder oiliness is increased after broken wall, and material is tacky, causes packaging difficult, reduction is usually required in actual production broken Wall rate improves mobility to reduce oozing out for oil, or addition auxiliary material such as microcrystalline cellulose, starch etc., and conidia powder quality is beaten greatly Discount;
3, taking in mode, if directly taking conidia powder, the special mouthfeel that conidia powder has allows some people to be difficult to connect By, and directly take there is certain excitant to stomach, hydrochloric acid in gastric juice also has certain destructiveness to conidia powder, and influence is absorbed;If straight Connect swallowable capsule, although the problem of solving mouthfeel, but long-term intake capsule can increase the extra burden of body.
2nd, except traditional ganoderma spove powder, to improve the utilization ratio of conidia powder, actual production also has one in managing A little conidia powder deep processed products, it can be common that lucidum spore powder water extract and ganoderma lucidum spore oil.Conidia powder water extract is main What is represented is water miscible active component in lucidum spore powder, such as polysaccharide, polypeptide, amino acid;What ganoderma lucidum spore oil was then included It is fat-soluble functional component in Reishi sporule, such as linoleic acid, leukotrienes, part triterpene, these products are unilaterally It make use of the functional component of conidia powder.Want intactly to absorb whole functional components of conidia powder, then need various product Take together.However, in view of the physical property of conidia powder water extract, spore oil and other extracts is different, if simply simply mixing Close, the mixture of paste is for filling, accumulating, to take be a problem and easily putrid and deteriorated, in addition it is also necessary to anti-by addition The compositions such as rotten agent extend the shelf life.At present, also no appearance by all active ingredient high efficiency extractions in conidia powder and can be fused into One possesses and has that accumulating is convenient, take simple, efficient quality guaranteeing and the high formulation of utilization rate and product concurrently.
Recently, the conidia powder product of " going wall conidia powder " concept has been got by some businessmans, but carefully studies discovery, its essence Simply using the dried powder of the water extract of conidia powder as " removing wall " conidia powder, its recovery rate is general in 20% or so, spore The active material that 30-40% is there remains in sub- powder is not utilized, therefore, be not truly remove wall Reishi sporule Powder.
Therefore, it is an object of the invention to prepare a lucidum spore powder truly to remove wall product, and formulation is excellent Good, storage is convenient, convenient to take, and the utilization rate of conidia powder is high.
The content of the invention
To overcome the deficiencies in the prior art, the whole effects of lucidum spore powder can be included it is an object of the invention to provide one kind Composition, the total ganoderma spore powder for having multiple advantage concurrently again removes wall micropill and preparation method thereof.Made micropill completely remains spore Whole functional components of powder, and packaging is convenient, it is easy to carry beneficial to taking, do not destroyed by hydrochloric acid in gastric juice, absorption rate is significantly carried Height, whole preparation technology is simple to operation.Micropill can also be matched somebody with somebody by adjusting the quality of Ganoderma spore extract and ganoderma lucidum spore oil Than being made rich in polysaccharide, removing wall series of products rich in the enhanced type conidia powder such as triterpene.
The technical scheme is that:By lucidum spore powder successively with food-grade liquid carbon dioxide, 95%, 75%, 50% concentration ethanol, water are extracted, and after extract is mixed in proportion, are mixed with 0.5%-5 weight % sodium alginate soln Uniformly, instill in 0.5-5 weight % calcium chloride water, form calcium alginate microsphere;The microballoon of formation soaks 1-240 minutes After take out, pure water clean up after dry, that is, obtain total ganoderma spore powder and remove wall micropill.
Sodium alginate, is the natural polymer extracted from sea-tangle, bulk kelp, with good bioadhesive with And compatibility, it is widely used in the industries such as food, medicine, daily use chemicals.Sodium alginate carries anion, can be with bivalent cation such as The insoluble alginic acid gel microsphere of the reaction production such as calcium ion, zinc ion, whole reaction condition is gentle, is extremely suitable for big point The absorption and embedding of sub- bioactive substance.The alginic acid gel microsphere of formation, is swelled in alkali, and insoluble in water and acid It is swollen, therefore active material can be avoided to be acid hydrolysis destruction, reduce stimulation of some compositions to stomach, at the same can also realize activity into Parcel, transmission and the sustained release divided, improves absorption rate.
Specifically, present invention offer is a kind of prepares formula and its method that total ganoderma spore powder removes wall micropill.It is described complete Lucidum spore powder removes the carbon dioxide abstraction thing that the active component of wall micropill is the lucidum spore powder being embedded in micropill shell, ethanol Extract and water extract, wherein the part by weight of the carbon dioxide abstraction thing, ethanol extract and water extract is 3-4 ∶1∶3-4.Wherein described micropill shell is by alginic acid gel-forming.Also, the total ganoderma spore powder goes wall micropill to pass through including under It is prepared by the method for stating step:
(1) under the conditions of 25-45 DEG C, 25-35MPa, with food-grade liquid carbon dioxide extracting ganoderma conidia powder, collection is obtained Obtain carbon dioxide abstraction thing (i.e. spore oil), isolated filter residue 1;
(2) filter residue 1 is successively extracted with 95% ethanol, 75% ethanol, 50% ethanol of 1-15 times of weight at 60 DEG C respectively 1-5 hours, collect and obtain ethanol extract, isolated filter residue 2;
(3) the last hot water with 1-20 times of weight of filter residue 2 is extracted 1-4 hours at 100 DEG C, collects and obtain hot water extraction Thing;
(4) the extraction product of step (1)-(3) and extract are merged, the viscosity with 0.5%-5 weight % is 20- 800cps sodium alginate aqueous solution mixing, is stirred while in droplets, dripping to 0.5-5 weight % calcium chloride water In solution, microspheric granula is formed, the microspheric granula formed soaks 1-240 points in 0.5-5 weight % calcium chloride water Zhong Hou, takes out, after being cleaned up in distilled water, dries, obtains total ganoderma spore powder and remove wall micropill.
Above step (1)-(3) are successively carried out, it is ensured that in conidia powder all active materials according to polarity from low to high Order is fully extracted, and the extracting substance of step (1)-(3) is merged, that is, represents conidia powder except all after exine shell Active ingredient, hereon referred to as " ganoderma spore powder extracts ".According to carbon dioxide abstraction thing, ethanol extract in conidia powder with And the content ratio of water extract, the three kinds of extracts prepared in advance also can be directly taken, after 3-4: 1: 3-4 proportions " ganoderma spore powder extracts " are prepared into, the natural ratio of effect material in conidia powder is reduced with this.Wherein, step (1) is obtained The carbon dioxide abstraction thing arrived is spore oil, and the conidia powder hot water extract of step (3) is also referred to as " conidia powder water in the present invention Extract ".In order to which " spore oil " that is obtained with step (1) is distinguished, below by step (2) and the conidia powder ethanol extract of (3) Spore powder extracts are collectively referred to as with water extract.In other words, in this manual, term " spore powder extracts " refers to by upper State the mixture of ethanol extract that step (2) and (3) obtain and water extract;Term " ganoderma spore powder extracts " refers to Spore oil (that is, carbon dioxide abstraction thing), ethanol extract and the water extract obtained by above-mentioned steps (1) (2) (3) it is mixed Compound.
In step (4), the sodium alginate for taking viscosity to be 20-800cps, it is 0.5%-5 weights that concentration is dissolved into distilled water Measure % sodium alginate aqueous solution.Sodium alginate has the ability for occurring gel reaction with bivalent cation, when being mixed with marine alga After the ganoderma spore powder extracts of sour sodium are contacted with calcium chloride, the gel network of network structure is formed on surface rapidly, will be complete Reishi sporule powder extracts are included in gel microsphere shell.
In the preparation process in accordance with the present invention, to the sodium alginate that is used in step (4), there is no particular limitation, as long as it is Viscosity meets limited range, and is the sodium alginate of food-grade or pharmaceutical grade, and (example at ambient temperature Such as, 20-30 DEG C) use.Usually, sodium alginate used can be 200,400 or 600cps in the viscosity of room temperature.
In a preferred embodiment, the viscosity of the sodium alginate used in step (4) is 200cps, sea used The concentration of alginic acid sodium water solution is 0.5 or 1 weight %.
In a preferred embodiment, the viscosity of the sodium alginate used in step (4) is 400cps, sea used The concentration of alginic acid sodium water solution is 0.5 weight %.
In a preferred embodiment, the viscosity of the sodium alginate used in step (4) is 600cps, sea used The concentration of alginic acid sodium water solution is 1 weight %.
Spore oil, conidia powder ethanol extract and water extract in step (1)-(3) can according to this area routine It is prepared by method.In addition, the inventors discovered that method, which is prepared as follows, can obtain the higher spore oil of recovery rate, conidia powder ethanol Extract or water extract:
More specifically, the preparation method (that is, the method that conidia powder is extracted with liquid carbon dioxide) of spore oil is as follows:
1. ganoderma spove powder is put into extraction kettle;
2. being pumped into liquid carbon dioxide, 40 DEG C of extraction kettle temperature, pressure 28MPa extractions are kept;
3. adjust 40 DEG C of the temperature of separation chamber 1, pressure 8MPa, 40 DEG C of the temperature of separation chamber 2, pressure 5MPa;
4. extraction 3.5 hours, collects the spore oil extracted, residue 1 is separated.
The preparation method of conidia powder ethanol extract is as follows:
1. above liquid carbon dioxide is extracted into ganoderma spove powder residue 1 remaining after spore oil is put into extraction vessel In;
2. extracted 2 hours under the conditions of adding 95% ethanol of 10 times of weight, 60 DEG C, filtering;
3. residue continues to extract 2 hours under the conditions of 75% ethanol with 10 times of weight, 60 DEG C, filtering;
4. residue continues to extract 2 hours under the conditions of 50% ethanol with 10 times of weight, 60 DEG C, filtering;
5. merging 3 filtrates, concentration obtains conidia powder ethanol extract after dry, pulverize, while separating residue 2.
The preparation method of conidia powder hot water extract is as follows:
1. the spore powder with crushed sporoderm residue 2 that above ethanol is extracted after conidia powder is put into extraction vessel;
2. extracted 2 hours under the conditions of adding the distilled water of 10 times of weight, 100 DEG C, filtering;
3. residue continues to extract 2 hours under the conditions of the distilled water with 10 times of weight, 100 DEG C, filtering;
4. merging 2 filtrates, concentration obtains conidia powder hot water extract and (is also referred to as in the present invention after dry, pulverize " conidia powder water extract ").
All extracts prepared by three of the above extracting process are well mixed, that is, represent included in conidia powder all Active ingredient, hereon referred to as " ganoderma spore powder extracts ", remaining residue is conidia powder wall.
In a preferred embodiment, step (4) miospore powder ethanol extract, water extract and spore oil is mixed The part by weight of compound and sodium alginate soln is in the range of 1: 1 to 1: 10, for example, can be 1: 1.5,1: 2,1: 3,1: 10 Deng.
In a preferred embodiment, the concentration of the calcium chloride water used in step (4) can be 1 weight Measure %, 2 weight %, 3 weight % or 4 weight %.The time that microspheric granula soaks in calcium chloride water can be 30 points Clock, 60 minutes, 120 minutes or 200 minutes.
In addition, it should be appreciated by those skilled in the art that can also be matched somebody with somebody in preparation process by adjusting each extract quality Than removing wall series of products with the enhanced type conidia powder being made rich in polysaccharide or rich in triterpene.When carbon dioxide abstraction thing, ethanol Extract and water extract by 3-4: 1: 3-4 part by weight proportioning when, can substantially reduce natural glossy ganoderma spore into Isloation state, while such mixture eliminates conidial cell wall, is conducive to absorbing.Lucidum spore powder water extract is rich in ganoderma lucidum Polysaccharide, lucidum spore powder ethanol extract is rich in ganoderma lucidum triterpene compounds, when the addition of increase lucidum spore powder water extract Ratio, can prepare the enhanced type conidia powder for obtaining being rich in polysaccharide and remove wall series of products;When increase lucidum spore powder alcohol extracting thing Adding proportion, can prepare and obtain the enhanced type conidia powder rich in triterpene and remove wall series of products.Meanwhile, those skilled in the art It should be understood that when the mass fraction increase of ganoderma lucidum spore oil, the mixture of Reishi sporule powder extracts and ganoderma lucidum spore oil into Ball is reduced, and is unfavorable for micropill shaping.The present invention is to the quality proportioning of Reishi sporule powder extracts and ganoderma lucidum spore oil without spy Do not limit, the need for those skilled in the art can be according to application, reasonable adjusting Reishi sporule powder extracts and ganoderma lucidum spore oil Quality proportioning.But preferably, substantially to reduce the carbon dioxide abstraction thing into isloation state of natural glossy ganoderma spore: ethanol is carried Take thing: water extract is that 3-4: 1: 3-4 (weight ratio) is prepared, and the bioavilability for removing wall micropill product so obtained is carried It is high.For example, the total ganoderma spore powder in the present invention is gone in wall micropill, it is embedded in carbon dioxide in the active component in micropill shell and extracts Take thing (i.e. ganoderma lucidum spore oil): ethanol extract: water extract (weight ratio) can be 3.6: 1: 3.6,3.5: 1: 3.8,4: 1: 3.3 wait.Those skilled in the art can be in the range of 3-4: 1: 3-4 part by weight to carbon dioxide abstraction thing (i.e. ganoderma lucidum spore Seed oil), ethanol extract:Reasonable adjustment is carried out with the content of water extract.Also, it will be appreciated by those skilled in the art that When preparation removes wall series of products rich in polysaccharide or the enhanced type conidia powder rich in triterpene, the active component in micropill shell is embedded in Middle carbon dioxide abstraction thing (i.e. ganoderma lucidum spore oil): ethanol extract: water extract (weight ratio) is not limited to the above, Ke Yiwei 3.6: 1: 12,1: 2.5: 1 etc., and those skilled in the art can need to fit above-mentioned part by weight according to actual product When adjustment.
In summary, the present invention provides following technical proposals:
1. a kind of total ganoderma spore powder removes wall micropill, its active component is the two of the lucidum spore powder being embedded in micropill shell Carbonoxide extract (i.e. ganoderma lucidum spore oil), ethanol extract and water extract, wherein the carbon dioxide abstraction thing, ethanol are carried The part by weight for taking thing and water extract is 3-4: 1: 3-4.
2. the total ganoderma spore powder according to the 1st removes wall micropill, it is prepared by the method comprised the steps::
(1) at 25-45 DEG C, 25-35MPa, with food-grade liquid carbon dioxide extracting ganoderma conidia powder, collects two obtained Carbonoxide extract, the carbon dioxide abstraction thing is spore oil, isolated filter residue 1;
(2) filter residue 1 is successively extracted with 95% ethanol, 75% ethanol, 50% ethanol of 1-15 times of weight at 60 DEG C respectively 1-5 hours, collect and obtain ethanol extract, isolated filter residue 2;
(3) the last hot water with 1-20 times of weight of filter residue 2 is extracted 1-4 hours at 100 DEG C, collects and obtain hot water extraction Thing;
(4) the extraction product of step (1)-(3) and extract are merged, the viscosity with 0.5%-5 weight % is 20- 800cps sodium alginate aqueous solution mixing, is stirred while in droplets, dripping to 0.5-5 weight % calcium chloride water In solution, microspheric granula is formed, the microspheric granula formed soaks 1-240 points in 0.5-5 weight % calcium chloride water Zhong Hou, takes out, after being cleaned up in distilled water, dries, obtains total ganoderma spore powder and remove wall micropill.
3. the total ganoderma spore powder according to the 2nd removes wall micropill, wherein in step (4), and the step (1) after merging- (3) product mixtures and the weight ratio of sodium alginate aqueous solution are 1: 1 to 1: 10.
4. the total ganoderma spore powder according to the 2nd removes wall micropill, wherein in step (4), and the step (1) after merging- (3) extraction product and the weight ratio of sodium alginate aqueous solution is 1: 1.5,1: 2,1: 3 or 1: 10.
5. the total ganoderma spore powder according to the 2nd removes wall micropill, sodium alginate used is in room wherein in step (4) The viscosity of temperature is 200,400 or 600cps.
6. the total ganoderma spore powder according to the 2nd removes wall micropill, the sodium alginate wherein used in step (4) is water-soluble The concentration of liquid is 0.5 weight % or 1 weight %.
7. the total ganoderma spore powder according to the 2nd removes wall micropill, the sodium alginate wherein used in step (4) it is glutinous Spend for 200cps, the concentration of sodium alginate aqueous solution used is 0.5 or 1 weight %.
8. the total ganoderma spore powder according to the 2nd removes wall micropill, the sodium alginate wherein used in step (4) it is glutinous Spend for 400cps, the concentration of sodium alginate aqueous solution used is 0.5 weight %.
9. the total ganoderma spore powder according to the 2nd removes wall micropill, the sodium alginate wherein used in step (4) it is glutinous Spend for 600cps, the concentration of sodium alginate aqueous solution used is 1 weight %.
10. the total ganoderma spore powder according to the 2nd removes wall micropill, the calcium chloride wherein used in step (4) is water-soluble The concentration of liquid is 1 weight %, 2 weight %, 3 weight % or 4 weight %, and the microspheric granula soaks in calcium chloride water The time of bubble is 30 minutes, 60 minutes, 120 minutes or 200 minutes.
11. the total ganoderma spore powder according to the 2nd removes wall micropill, its is spherical in shape or subsphaeroidal, a diameter of 2.9- 3.3mm。
12. the total ganoderma spore powder according to the 2nd removes wall micropill, it maintains the original state in gastric juice, the 2-3 in intestinal juice It is swelled after hour until disintegration.
13. the total ganoderma spore powder according to the 2nd removes wall micropill, wherein conidia powder utilization rate is more than 95%.
14. the total ganoderma spore powder according to the 2nd removes wall micropill, wherein in the active component being embedded in micropill shell Carbon dioxide abstraction thing (i.e. ganoderma lucidum spore oil): ethanol extract: water extract (weight ratio) is 3.6: 1: 3.6.
15. the total ganoderma spore powder according to the 2nd removes wall micropill, wherein in the active component being embedded in micropill shell Carbon dioxide abstraction thing (i.e. ganoderma lucidum spore oil): ethanol extract: water extract (weight ratio) is 3.5: 1: 3.8.
16. the total ganoderma spore powder according to the 2nd removes wall micropill, wherein in the active component being embedded in micropill shell Carbon dioxide abstraction thing (i.e. ganoderma lucidum spore oil): ethanol extract: water extract (weight ratio) is 4: 1: 3.3.
The beneficial effects of the invention are as follows:
1. the method for the present invention is truly realizing that conidia powder removes wall, the powerful material of institute in conidia powder is completely protected Stay and concentrate on a formulation, abandon useless conidial cell wall.Effect material proportion brings up to more than 95% (containing micro by 50% or so Calcium alginate), solve the problem of common conidia powder effect material utilization is low;
2. in the equivalent using upper of conidia powder, take the present invention and go wall micropill about 1g to can reach the effect for taking 2g conidia powders Really, dose halves;
3. ganoderma lucidum spore oil is embedded in micropill, oxidation becomes caused by solving common spore powder with crushed sporoderm miospore oil extravasation The problem of matter;
4. made micropill physical toughness is good, mobility is good, solves spore powder with crushed sporoderm spore oil and oozes out caused material hair Viscous, not easy to package the problem of;
5. micropill is easy to swallow, poor taste caused by oral powder is solved the problems, such as;
6. prepared by the active material bearing capacity originated to conidia powder of micropill it is strong, micropill is steady in simulated person's work gastric juice Release is disintegrated in fixed, intestinal juice, the problem of solving the gastric irritation of common spore powder with crushed sporoderm presence and decomposed by gastric juice.
Except the functional component of the reduction original ratio of conidia powder, richness can also be prepared into by adjusting the ratio of each extract The enhanced type lucidum spore powder of polysaccharide, rich triterpene etc. removes wall pellet preparations.
Brief description of the drawings
From detailed description below in conjunction with the accompanying drawings, features described above and advantage of the invention will be apparent from, wherein:
Fig. 1 show the embodiment of the present invention 2 prepare go wall micropill simulate the gastric juice 0.1mol/L hydrochloric acid solutions (HCl, PH1.0 the photo of 3 hours) is swelled in the phosphate buffer (PBS, pH7.4) (B) of (A) and simulated intestinal fluid.
Fig. 2 show the embodiment of the present invention 2 prepare go wall micropill simulate the gastric juice 0.1mol/L hydrochloric acid solutions (HCl, PH1.0 the photo of 12 hours) is swelled in the phosphate buffer (PBS, pH7.4) (B) of (A) and simulated intestinal fluid.
Prepared by Fig. 3 display embodiment of the present invention 2 goes swelling ratio curve of the wall micropill in different medium (to be swelled rear microballoon External diameter is with being swelled preceding dry microspheres external diameter ratio, 100%).
Embodiment
The present invention is further described referring to specific embodiment, it will be appreciated by those skilled in the art that this hair It is bright to be not limited to these specific embodiments.
The preparation of the Reishi sporule powder extracts of embodiment 1. and spore oil
Reishi sporule powder extracts and spore oil for the present invention can be prepared according to the conventional method of this area, generally Selection and withdrawal rate is more than 15-20% spore oil, and more than 5% ethanol extract, more than 15-20% water extract is used for The present invention.If without specified otherwise, " alcohol extracting thing " of conidia powder generally refers to the ethanol extract of conidia powder.
In addition, the inventors discovered that method, which is prepared as follows, can obtain the higher spore oil of recovery rate, conidia powder alcohol extracting Take thing or water extract:
The preparation method (that is, the method that conidia powder is extracted with liquid carbon dioxide) of spore oil is as follows:
1. ganoderma spove powder is put into extraction kettle;
2. being pumped into liquid carbon dioxide, 40 DEG C of extraction kettle temperature, pressure 28MPa extractions are kept;
3. adjust 40 DEG C of the temperature of separation chamber 1, pressure 8MPa, 40 DEG C of the temperature of separation chamber 2, pressure 5MPa;
4. extraction 3.5 hours, collects the spore oil extracted, residue 1 is separated.
The preparation method of conidia powder ethanol extract is as follows:
1. above liquid carbon dioxide is extracted into ganoderma spove powder residue 1 remaining after spore oil is put into extraction vessel In;
2. extracted 2 hours under the conditions of adding 95% ethanol of 10 times of weight, 60 DEG C, filtering;
3. residue continues to extract 2 hours under the conditions of 75% ethanol with 10 times of weight, 60 DEG C, filtering;
4. residue continues to extract 2 hours under the conditions of 50% ethanol with 10 times of weight, 60 DEG C, filtering;
5. merging 3 filtrates, concentration obtains conidia powder ethanol extract after dry, pulverize, while separating residue 2.
The preparation method of conidia powder hot water extract is as follows:
1. the spore powder with crushed sporoderm residue 2 that above ethanol is extracted after conidia powder is put into extraction vessel;
2. extracted 2 hours under the conditions of adding 10 times of weight distilled water, 100 DEG C, filtering;
3. residue continues to use 10 times of weight distilled water, extract 2 hours under the conditions of 100 DEG C, filter;
4. merging 2 filtrates, concentration obtains conidia powder hot water extract and (is also referred to as in the present invention after dry, pulverize " conidia powder water extract ").
All extracts prepared by three of the above extracting process are well mixed, and can also be extracted ganoderma lucidum spore oil, ethanol Thing and lucidum spore powder water extract are mixed by its natural ratio, i.e. 3-4: 1: 3-4 (weight ratio) in conidia powder, i.e. generation All active ingredients included in table conidia powder, are herein collectively referred to as after " ganoderma spore powder extracts ", water hot extraction remaining Residue be conidia powder wall.
The product referred to as spore oil that conidia powder is obtained is extracted with liquid carbon dioxide, is extracted with alcohol extraction liquid state carbon dioxide The product that residue after taking is obtained is referred to as conidia powder ethanol extract, the product that the residue after being extracted with water hot extraction's ethanol is obtained Referred to as conidia powder hot water extract (also referred to as conidia powder water extract).In order to be distinguished with spore oil, conidia powder ethanol is extracted The mixture of thing and conidia powder water extract is collectively referred to as spore powder extracts.And by spore oil, conidia powder ethanol extract and spore Sub- powder water extract merges obtained mixture and is referred to as " ganoderma spore powder extracts ".
The micropill preparation example 1 of embodiment 2.
Take spore oil 4.4g, ethanol extract 1.2g, the water extract 4.4g of the method preparation according to embodiment 1, i.e., it is complete Reishi sporule powder extracts 10g, wherein spore oil: ethanol extract: the part by weight of water extract is about 3.6: 1: 3.6, with The sodium alginate soln that 20g concentration is 0.5 weight %, viscosity is 200cps (room temperature) (for 200cps sodium alginate purchase by viscosity Self-evident moon marine alga group) it is mixed and stirred for uniformly, treating dissipation of air bubbles, it is 1 slowly to drip to concentration in droplets while stirring In weight % calcium chloride solution, after soaking 30 minutes, micropill is taken out, is totally dried afterwards with distilled water flushing, obtains finished product Micropill.
Obtained micropill is spherical in shape, subsphaeroidal, and a diameter of 3.0-3.2mm, weight is 18.5-19.0mg.
Whole preparation process needs sterile, used water, sodium alginate soln, calcium chloride solution to be required to be sterile.
The micropill preparation example 2 of embodiment 3.
Take spore oil 4.2g, ethanol extract 1.2g, the water extract 4.6g of the method preparation according to embodiment 1, i.e., it is complete Reishi sporule powder extracts 10g, wherein spore oil: ethanol extract: the part by weight of water extract is about 3.5: 1: 3.8, with The sodium alginate soln that 15g concentration is 0.5 weight %, viscosity is 400cps (room temperature) (for 400cps sodium alginate purchase by viscosity Self-evident moon marine alga group) it is mixed and stirred for uniformly, treating dissipation of air bubbles, it is 3 slowly to drip to concentration in droplets while stirring In weight % calcium chloride solution, after soaking 30 minutes, micropill is taken out, is totally dried afterwards with distilled water flushing, obtains finished product Micropill..
Obtained micropill is spherical in shape, subsphaeroidal, and a diameter of 2.9-3.0mm, weight is 17.8-18.5mg.
Whole preparation process needs sterile, used water, sodium alginate soln, calcium chloride solution to be required to be sterile.
The micropill preparation example 3 of embodiment 4.
Take spore oil 4.8g, ethanol extract 1.2g, the water extract 4.0g of the method preparation according to embodiment 1, i.e., it is complete Reishi sporule powder extracts 10g, wherein spore oil: ethanol extract: the part by weight of water extract is about 4: 1: 3.3, with 30g (viscosity is purchased from bright moon to the sodium alginate soln that concentration is 1 weight %, viscosity is 600cps (room temperature) for 600cps sodium alginate Marine alga group) it is mixed and stirred for uniformly, treating dissipation of air bubbles, concentration is slowly dropped into droplets while stirring for 2 weight % Calcium chloride solution in, immersion 60 minutes after, micropill is taken out, is totally dried afterwards with distilled water flushing, obtains finished product micropill.
Obtained micropill is spherical in shape, subsphaeroidal, and a diameter of 3.1-3.3mm, weight is 21.0-21.5mg.
Whole preparation process needs sterile, used water, sodium alginate soln, calcium chloride solution to be required to be sterile.
Above example 2-4 is matched by the natural ratio of each extract of conidia powder miospore powder, and prepared is micro- Ball is to represent the powerful material of conidia powder institute after shelling, if desired prepares the micropill of reinforcing polysaccharide or triterpene, then can pass through Prepared by regulation proportioning, be specifically shown in following examples:
The micropill preparation example 4 of embodiment 5.
The conidia powder of reinforcing polysaccharide removes wall micropill:Spore oil 4.4g, ethanol extract 1.2g, water extract 4.4g are taken, i.e., Ganoderma spore powder extracts 10g, wherein spore oil: ethanol extract: the part by weight of water extract is about 3.6: 1: 3.6, Separately plus 10g conidia powders water extract (is prepared, now wherein spore oil: ethanol extract: water is extracted as described in Example 1 The part by weight of thing is about 3.6: 1: 12), with the sodium alginate soln that 60g concentration is 1 weight %, viscosity is 200cps (room temperature) (viscosity is purchased from bright moon marine alga group for 200cps sodium alginate) is mixed and stirred for uniform, treats dissipation of air bubbles, while stirring with The form of drop is slowly dripped in the calcium chloride solution that concentration is 4 weight %, after soaking 120 minutes, micropill is taken out, with distillation Water is dried after rinsing well, obtains finished product micropill.
Obtained micropill is spherical in shape, subsphaeroidal, and a diameter of 3.2-3.3mm, weight is 22.5-23.0mg.
Whole preparation process needs sterile, used water, sodium alginate soln, calcium chloride solution to be required to be sterile.
The micropill preparation example 5 of embodiment 6.
The conidia powder of reinforcing triterpene removes wall micropill:Spore oil 4.4g, ethanol extract 1.2g, water extract 4.4g are taken, i.e., Ganoderma spore powder extracts 10g, wherein spore oil: ethanol extract: the part by weight of water extract is about 3.6: 1: 3.6, Separately plus 10g conidia powders ethanol extract (is prepared, now wherein spore oil: ethanol extract: water extraction as described in Example 1 The part by weight for taking thing is about 1: 2.5: 1), molten with 200g concentration is 1 weight %, viscosity is 200cps (room temperature) sodium alginate Liquid (viscosity is purchased from bright moon marine alga group for 200cps sodium alginate) is mixed and stirred for uniformly, treating dissipation of air bubbles, while stirring Slowly drip in the calcium chloride solution that concentration is 1 weight %, after soaking 200 minutes, micropill is taken out, with steaming in droplets Distilled water is dried after rinsing well, obtains finished product micropill.
Obtained micropill is spherical in shape, subsphaeroidal, and a diameter of 3.2-3.3mm, weight is 22.5-23.0mg.
Whole preparation process needs sterile, used water, sodium alginate soln, calcium chloride solution to be required to be sterile.
Prepared by the present invention of embodiment 7. removes wall micropill and conidia powder, the comparison of common " removing wall " product
Common " remove wall " product of the wall micropill with being currently known in conidia powder, this area is gone to carry out by prepared by embodiment 2 Compare.
Described common " removing wall " product refer in this area it is common at present merely with lucidum spore powder water extract, without The Related product developed containing any ganoderma lucidum spore oil and lucidum spore powder alcohol extracting thing, for example, be distributed into pouch or be filled into Capsule.
Prepared by the present invention of table 1. goes wall micropill and the sense organ of conidia powder, common " removing wall " product to be compared
From table 1, prepared by the present invention removes wall micropill compared with common " removing wall " and common spore powder with crushed sporoderm product Compared with good fluidity, filling convenience, taking the good integrated sensory's feature of convenient, palatability.
Prepared by the present invention of table 2. goes wall micropill and the utilization rate of conidia powder, common " removing wall " product to be compared
From table 2, although the nutritional ingredient in conidia powder can all be absorbed by taking common conidia powder, but due to broken wall It is useless conidial cell wall that conidia powder, which contains 40-50%, therefore only make use of wherein 50-60% or so active principle;Commonly " removing wall " product essence is the hot water extract of lucidum spore powder, and representative is functional component based on polysaccharide, not comprising spore Seed oil and alcohol extracting thing, therefore only make use of the active ingredient of 15-20% in conidia powder;And the present invention prepare remove wall micropill, Active ingredients all in conidia powder are contained, product is free of any conidial cell wall, and conidia powder utilization rate reaches more than 95% (deduction Extract the part of loss and micro calcium alginate), utilization rate is greatly improved.
In addition, removing 0.1mol/L hydrochloric acid solution of the wall micropill respectively in simulate the gastric juice by prepared by embodiments of the invention 2 Be swelled in the phosphate buffer (PBS, pH7.4) (Figure 1B, 2B) of (HCl, pH1.0) (Figure 1A, 2A) and simulated intestinal fluid 3 hours, 12 hours, and draw corresponding swelling ratio (being swelled rear microballoon external diameter and dry microspheres external diameter ratio, 100% before being swelled) curve, As a result it is shown in Fig. 1,2,3.
Fig. 1-3 illustrates that the present invention prepares micropill and maintained the original state in gastric juice, is swelled in intestinal juice after 2-3 hours until collapsing Solution, therefore active ingredient can be protected not destroyed by hydrochloric acid in gastric juice, directly absorbed into enteron aisle.
It should be understood that although with reference to its exemplary embodiment, particularly shown and description is carried out to the present invention, It should be understood by those skilled in the art that without departing substantially from spirit of the invention as defined in appended claims Under conditions of scope, the change of various forms and details can be carried out wherein, any of various embodiments can be carried out Combination.

Claims (13)

1. a kind of total ganoderma spore powder removes wall micropill, its active component is the titanium dioxide for the lucidum spore powder being embedded in micropill shell Carbon extract, ethanol extract and water extract, wherein the carbon dioxide abstraction thing, ethanol extract and water extract Part by weight is 3-4: 1: 3-4.
2. total ganoderma spore powder according to claim 1 removes wall micropill, it is prepared by the method comprised the steps:
(1) at 25-45 DEG C, 25-35MPa, with food-grade liquid carbon dioxide extracting ganoderma conidia powder, collects the titanium dioxide obtained Carbon extract, the carbon dioxide abstraction thing is spore oil, isolated filter residue 1;
(2) it is filter residue 1 is small in 60 DEG C of priority extraction 1-5 with 95% ethanol, 75% ethanol, 50% ethanol of 1-15 times of weight respectively When, collect and obtain ethanol extract, isolated filter residue 2;
(3) the last hot water with 1-20 times of weight of filter residue 2 is extracted 1-4 hours at 100 DEG C, collects and obtain hot water extract;
(4) the extraction product of step (1)-(3) and extract are merged, the viscosity with 0.5%-5 weight % is 20-800cps's Sodium alginate aqueous solution is mixed, and is stirred while in droplets, in the calcium chloride water for dripping to 0.5-5 weight %, Microspheric granula is formed, after the microspheric granula formed soaks 1-240 minutes in 0.5-5 weight % calcium chloride water, is taken Go out, after being cleaned up in distilled water, dry, obtain total ganoderma spore powder and remove wall micropill.
3. total ganoderma spore powder according to claim 2 removes wall micropill, wherein in step (4), and the step (1) after merging- (3) product mixtures and the weight ratio of sodium alginate aqueous solution are 1: 1 to 1: 10.
4. total ganoderma spore powder according to claim 2 removes wall micropill, wherein in step (4), and the step (1) after merging- (3) product mixtures and the weight ratio of sodium alginate aqueous solution are 1: 1.5,1: 2,1: 3 or 1: 10.
5. total ganoderma spore powder according to claim 2 removes wall micropill, sodium alginate used is in room wherein in step (4) The viscosity of temperature is 200,400 or 600cps.
6. total ganoderma spore powder according to claim 2 removes wall micropill, the sodium alginate wherein used in step (4) is water-soluble The concentration of liquid is 0.5 weight % or 1 weight %.
7. total ganoderma spore powder according to claim 2 removes wall micropill, the sodium alginate wherein used in step (4) it is glutinous Spend for 200cps, the concentration of sodium alginate aqueous solution used is 0.5 or 1 weight %.
8. total ganoderma spore powder according to claim 2 removes wall micropill, the sodium alginate wherein used in step (4) it is glutinous Spend for 400cps, the concentration of sodium alginate aqueous solution used is 0.5 weight %.
9. total ganoderma spore powder according to claim 32 removes wall micropill, the sodium alginate wherein used in step (4) Viscosity is 600cps, and the concentration of sodium alginate aqueous solution used is 1 weight %.
10. total ganoderma spore powder according to claim 2 removes wall micropill, the calcium chloride wherein used in step (4) is water-soluble The concentration of liquid is 1 weight %, 2 weight %, 3 weight % or 4 weight %, and the microspheric granula soaks in calcium chloride water The time of bubble is 30 minutes, 60 minutes, 120 minutes or 200 minutes.
11. total ganoderma spore powder according to claim 2 removes wall micropill, its is spherical in shape or subsphaeroidal, a diameter of 2.9- 3.3mm。
12. total ganoderma spore powder according to claim 2 removes wall micropill, it maintains the original state in gastric juice, the 2-3 in intestinal juice It is swelled after hour until disintegration.
13. total ganoderma spore powder according to claim 2 removes wall micropill, wherein conidia powder utilization rate is more than 95%.
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