CN107158046B - A wall-removing pellet containing Ganoderma spore powder - Google Patents
A wall-removing pellet containing Ganoderma spore powder Download PDFInfo
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- CN107158046B CN107158046B CN201710511241.6A CN201710511241A CN107158046B CN 107158046 B CN107158046 B CN 107158046B CN 201710511241 A CN201710511241 A CN 201710511241A CN 107158046 B CN107158046 B CN 107158046B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/06—Fungi, e.g. yeasts
- A61K36/07—Basidiomycota, e.g. Cryptococcus
- A61K36/074—Ganoderma
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules 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
- A61K9/5005—Wall or coating material
- A61K9/5021—Organic macromolecular compounds
- A61K9/5036—Polysaccharides, e.g. gums, alginate; Cyclodextrin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction 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
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
Abstract
The invention provides a total ganoderma spore powder wall-removing pellet, which comprises active ingredients of a carbon dioxide extract, an ethanol extract and a water extract which are embedded in a pellet shell and contain ganoderma spore powder, wherein the weight ratio of the carbon dioxide extract, the ethanol extract and the water extract is 3-4: 1: 3-4. The total ganoderma lucidum spore powder wall-removing pellet is prepared by the following steps: mixing the liquid carbon dioxide extract, the ethanol extract and the water extract of the ganoderma spore powder, mixing with 0.5-5 wt% of sodium alginate aqueous solution with the viscosity of 20-800cps, dripping into 0.5-5 wt% of calcium chloride aqueous solution while stirring to form spherical pellets, soaking the formed spherical pellets in 0.5-5 wt% of calcium chloride aqueous solution for 1-240 minutes, taking out, cleaning in distilled water, and drying to obtain the wall-removed full ganoderma spore powder pellets.
Description
Technical Field
The invention relates to a total ganoderma lucidum spore powder wall-removing pellet and a preparation method thereof, belonging to the field of medicines.
Background
The ganoderma lucidum spore powder is the essence of ganoderma lucidum, contains rich bioactive components and has important medicinal health-care function. The main components of the ganoderma lucidum spore powder exerting the effects are a series of bioactive substances such as ganoderma lucidum polysaccharide, ganoderma lucidum triterpene and the like, the active substances are wrapped in hard spore walls, and only when the ganoderma lucidum spores are broken, the effective components can be released and utilized. According to modern separation and extraction technology, active substances with different characteristics in ganoderma spore powder need to be extracted by different extraction solvents, such as ganoderma spore oil extracted by food-grade liquid carbon dioxide, unsaturated fatty acid, ganoderma triterpene and other active ingredients can be extracted, triterpene and active substances with medium polarity can be extracted by ethanol extraction, and polysaccharides, polypeptides, amino acids and other substances of ganoderma are mainly extracted by hot water extraction. The three substances basically represent all effective substances contained in the spore powder, account for 50-60% of the spore powder, and the rest 40-50% of the spore powder is unavailable ganoderma lucidum spore wall.
The utilization of the ganoderma lucidum spore powder has the following two problems:
firstly, the traditional ganoderma lucidum spore powder is generally used after being directly subpackaged into small bags or filled into capsules after wall breaking, and has the following defects:
1, 1 part of spore powder product is taken, half of the spore powder product is ineffectiveness spore wall, only half of effective components are really absorbed, and the absorption utilization rate is low;
2, the oil property of the spore powder is increased after wall breaking, the materials are sticky, so that the packaging is difficult, the wall breaking rate is generally required to be reduced in the actual production to reduce the oil content seepage, or auxiliary materials such as microcrystalline cellulose, starch and the like are added to improve the fluidity, and the quality of the spore powder is greatly reduced;
3, in the aspect of taking, if the spore powder is directly taken, the special taste of the spore powder is unacceptable for some people, and the direct taking has certain irritation to stomach, and the gastric acid has certain destructiveness to the spore powder to influence absorption and utilization; if the capsule is swallowed directly, although the problem of taste is solved, the capsule is taken for a long time, which will increase the extra burden of the body.
Secondly, in addition to the traditional wall-broken ganoderma lucidum spore powder, in order to improve the utilization efficiency of the spore powder, some deep-processed products of the spore powder are also available in actual production and operation, and the water extract of the ganoderma lucidum spore powder and ganoderma lucidum spore oil are common. The spore powder water extract mainly represents water-soluble active ingredients in Ganoderma spore powder, such as polysaccharide, polypeptide, amino acids, etc.; the ganoderma lucidum spore oil contains fat-soluble functional components in ganoderma lucidum spores, such as linoleic acid, linolenic acid, partial triterpenes and the like, and the products only utilize the functional components of spore powder in a one-sided manner. In order to completely absorb and utilize all functional components of the spore powder, various products are required to be taken together. However, since the aqueous extract of spore powder, the spore oil and the other extracts have different physical properties, if they are simply mixed, the pasty mixture is difficult to fill, store and transport, and take, and is highly perishable, and it is necessary to prolong the shelf life by adding a component such as a preservative. At present, all effective components in spore powder can be efficiently extracted and fused into a dosage form and a product which have the advantages of convenient storage and transportation, simple administration, high efficiency and quality guarantee and high utilization rate.
Recently, some merchants have developed spore powder products with the concept of wall-removed spore powder, but careful researches have found that the essence of the spore powder is only that the powder obtained by drying the water extract of the spore powder is used as the wall-removed spore powder, the extraction rate is about 20 percent generally, and the remaining 30 to 40 percent of active substances in the spore powder are not utilized, so the spore powder is not wall-removed ganoderma lucidum spore powder in the true sense.
Therefore, the invention aims to prepare a ganoderma lucidum spore powder wall-removing product in the true sense, and the ganoderma lucidum spore powder wall-removing product has the advantages of excellent dosage form, convenience for storage and taking and high utilization rate of spore powder.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a total ganoderma spore powder wall-removing pellet which can contain all functional components of ganoderma spore powder and has multiple advantages and a preparation method thereof. The prepared pellet completely retains all functional components of spore powder, is convenient to package, take and carry, is not damaged by gastric acid, greatly improves the absorption and utilization rate, and is simple and easy to operate in the whole preparation process. The pellet can also be prepared into enhanced spore powder wall-removed series products rich in polysaccharide, triterpene and the like by adjusting the mass ratio of the ganoderma lucidum spore extract to the ganoderma lucidum spore oil.
The technical scheme of the invention is as follows: sequentially extracting Ganoderma spore powder with food-grade liquid carbon dioxide, 95%, 75%, 50% ethanol and water, mixing the extracts at a certain proportion, mixing with 0.5-5 wt% sodium alginate solution, and dripping into 0.5-5 wt% calcium chloride water solution to form calcium alginate microspheres; soaking the formed microspheres for 1-240 min, taking out, cleaning with purified water, and drying to obtain the wall-removed total ganoderma spore powder micro-pill.
Sodium alginate is a natural high molecular compound extracted from kelp and kelp, has good biological adhesion and compatibility, and is widely applied to the industries of food, medicine, daily chemicals and the like. The sodium alginate carries anions, can react with divalent cations such as calcium ions, zinc ions and the like to produce insoluble alginate gel pellets, has mild reaction conditions, and is very suitable for adsorption and embedding of macromolecular bioactive substances. The formed alginic acid gel micro-pill swells in alkali but does not swell in water and acid, thereby avoiding the active substance from being destroyed by acidolysis, reducing the stimulation of certain components to the stomach, realizing the wrapping, transmission and slow release of the active components and improving the absorption and utilization rate.
Specifically, the invention provides a formula and a method for preparing a total ganoderma lucidum spore powder wall-removing pellet. The active ingredients of the whole ganoderma lucidum spore powder wall-removing pellet are a carbon dioxide extract, an ethanol extract and a water extract of ganoderma lucidum spore powder embedded in a pellet shell, wherein the weight ratio of the carbon dioxide extract, the ethanol extract and the water extract is 3-4: 1: 3-4. Wherein the pellet shell is formed from alginic acid gel. And the total ganoderma lucidum spore powder wall-removing pellet is prepared by the method comprising the following steps:
(1) extracting Ganoderma spore powder with food-grade liquid carbon dioxide at 25-45 deg.C and 25-35MPa, collecting to obtain carbon dioxide extract (spore oil), and separating to obtain residue 1;
(2) extracting the residue 1 with 1-15 times of 95% ethanol, 75% ethanol, and 50% ethanol at 60 deg.C for 1-5 hr, collecting ethanol extract, and separating to obtain residue 2;
(3) extracting the residue 2 with 1-20 times of hot water at 100 deg.C for 1-4 hr, and collecting to obtain hot water extract;
(4) mixing the extraction product and the extract obtained in the steps (1) - (3), mixing with 0.5-5 wt% of sodium alginate aqueous solution with the viscosity of 20-800cps, dripping into 0.5-5 wt% of calcium chloride aqueous solution while stirring to form spherical pellets, soaking the formed spherical pellets in 0.5-5 wt% of calcium chloride aqueous solution for 1-240 minutes, taking out, cleaning in distilled water, and drying to obtain the wall-removed full ganoderma spore powder pellets.
The steps (1) to (3) are carried out in sequence, so that all active substances in the spore powder are fully extracted according to the sequence of the polarity from low to high, and the extracted substances in the steps (1) to (3) are combined to represent all effective components of the spore powder after the spore shells are removed, and the effective components are called as 'total ganoderma lucidum spore powder extract'. According to the content ratio of the carbon dioxide extract, the ethanol extract and the water extract in the spore powder, three kinds of extracts prepared in advance can be directly taken and prepared into 'total ganoderma spore powder extract' according to the proportion of 3-4: 1: 3-4, so that the natural proportion of the effective substances in the spore powder is reduced. Wherein, the carbon dioxide extract obtained in the step (1) is spore oil, and the spore powder hot water extract obtained in the step (3) is also called as 'spore powder water extract' in the invention. In order to distinguish from the "spore oil" obtained in step (1), the combination of the ethanol extract and the water extract of the spore powder obtained in steps (2) and (3) is hereinafter referred to as spore powder extract. In other words, in the present specification, the term "spore powder extract" refers to a mixture of the ethanol extract and the water extract obtained by the above-mentioned steps (2) and (3); the term "whole ganoderma lucidum spore powder extract" refers to a mixture of the spore oil (i.e., carbon dioxide extract), ethanol extract and water extract obtained by the above steps (1) (2) (3).
In the step (4), sodium alginate with the viscosity of 20-800cps is dissolved into sodium alginate water solution with the concentration of 0.5-5 wt% by using distilled water. The sodium alginate has the capability of generating gel reaction with divalent cations, when the total ganoderma spore powder extract mixed with the sodium alginate contacts with calcium chloride, a gel network with a net structure is rapidly formed on the surface, and the total ganoderma spore powder extract is contained in the shell of the gel pellet.
In the preparation method of the present invention, there is no particular limitation on the sodium alginate used in step (4), as long as it is a sodium alginate that satisfies the defined range of viscosity and is food grade or pharmaceutical grade, and is used under room temperature conditions (e.g., 20 to 30 ℃). In general, sodium alginate may be used having a viscosity of 200, 400 or 600cps at room temperature.
In a preferred embodiment, the viscosity of sodium alginate used in step (4) is 200cps and the concentration of the aqueous sodium alginate solution used is 0.5 or 1% by weight.
In a preferred embodiment, the viscosity of sodium alginate used in step (4) is 400cps and the concentration of the aqueous sodium alginate solution used is 0.5% by weight.
In a preferred embodiment, the viscosity of sodium alginate used in step (4) is 600cps and the concentration of the aqueous sodium alginate solution used is 1% by weight.
The spore oil, the ethanol extract of spore powder and the water extract in steps (1) to (3) may be prepared according to a conventional method in the art. In addition, the inventor finds that the spore oil, the spore powder ethanol extract or the spore powder water extract with higher extraction rate can be obtained by the following preparation method:
more specifically, the method for preparing the spore oil (i.e., the method for extracting the spore powder with liquid carbon dioxide) is as follows:
1. putting the wall-broken ganoderma lucidum spore powder into an extraction kettle;
2. pumping liquid carbon dioxide, keeping the temperature of the extraction kettle at 40 ℃, and extracting under the pressure of 28 MPa;
3. adjusting the temperature of the separation chamber 1 to 40 ℃ and the pressure to 8MPa, and the temperature of the separation chamber 2 to 40 ℃ and the pressure to 5 MPa;
4. extracting for 3.5 hours, collecting extracted spore oil, and separating residue 1.
The preparation method of the spore powder ethanol extract comprises the following steps:
1. putting the residual wall-broken ganoderma lucidum spore powder residue 1 after extracting the spore oil by the liquid carbon dioxide into an extraction container;
2. adding 10 times of 95% ethanol, extracting at 60 deg.C for 2 hr, and filtering;
3. extracting the residue with 10 times of 75% ethanol at 60 deg.C for 2 hr, and filtering;
4. extracting the residue with 10 times of 50% ethanol at 60 deg.C for 2 hr, and filtering;
5. mixing the filtrates, concentrating, drying, pulverizing to obtain spore powder ethanol extract, and separating residue 2.
The preparation method of the spore powder hot water extract comprises the following steps:
1. putting the wall-broken spore powder residue 2 after extracting the spore powder by the ethanol into an extraction container;
2. adding 10 times of distilled water, extracting at 100 deg.C for 2 hr, and filtering;
3. extracting the residue with 10 times of distilled water at 100 deg.C for 2 hr, and filtering;
4. the filtrates were combined 2 times, concentrated, dried, and pulverized to obtain a hot water extract of spore powder (also referred to as "spore powder aqueous extract" in the present invention).
All the extracts prepared by the three extraction methods are uniformly mixed, namely all the effective components contained in the spore powder are represented, the extracts are called as 'total ganoderma lucidum spore powder extracts', and the residual residues are the spore powder walls.
In a preferred embodiment, the weight ratio of the mixture of the ethanol extract, the water extract and the spore oil of the spore powder to the sodium alginate solution in the step (4) is in the range of 1:1 to 1:10, for example, 1:1.5, 1:2, 1:3, 1:10, etc.
In a preferred embodiment, the concentration of the aqueous calcium chloride solution used in step (4) may be 1 wt%, 2 wt%, 3 wt%, or 4 wt%. The time for soaking the spherical pellets in the aqueous calcium chloride solution may be 30 minutes, 60 minutes, 120 minutes or 200 minutes.
In addition, as will be understood by those skilled in the art, the polysaccharide-rich or triterpene-rich fortified spore powder wall-removed series product can also be prepared by adjusting the mass ratio of each extract in the preparation process. When the carbon dioxide extract, the ethanol extract and the water extract are mixed according to the weight ratio of 3-4: 1: 3-4, the component state of the natural ganoderma lucidum spores can be basically reduced, and the spore walls of the mixture are removed, so that the mixture is favorable for absorption and utilization. The ganoderma lucidum spore powder water extract is rich in ganoderma lucidum polysaccharide, the ganoderma lucidum spore powder ethanol extract is rich in ganoderma lucidum triterpenoids, and when the adding proportion of the ganoderma lucidum spore powder water extract is increased, a series of products of polysaccharide-rich enhanced spore powder wall removal can be prepared; when the adding proportion of the alcohol extract of the ganoderma lucidum spore powder is increased, a series of products of wall removal of the enhanced spore powder rich in triterpene can be prepared. Meanwhile, it will be understood by those skilled in the art that, when the mass fraction of the ganoderma lucidum spore oil is increased, the pelleting property of the mixture of the ganoderma lucidum spore powder extract and the ganoderma lucidum spore oil is reduced, which is not favorable for pellet forming. The mass ratio of the ganoderma lucidum spore powder extract to the ganoderma lucidum spore oil is not particularly limited, and the technical personnel in the field can reasonably adjust the mass ratio of the ganoderma lucidum spore powder extract to the ganoderma lucidum spore oil according to the application requirement. Preferably, however, the carbon dioxide extract, ethanol extract and water extract are formulated in a weight ratio of 3-4: 1: 3-4 to substantially reduce the content of the natural Ganoderma lucidum spores, so that the bioavailability of the resulting de-walled pellet product is improved. For example, in the total ganoderma spore powder wall-removed pellet of the present invention, the weight ratio of the carbon dioxide extract (i.e. ganoderma spore oil) to the ethanol extract to the water extract (i.e. ganoderma spore oil) in the active ingredient embedded in the pellet shell may be 3.6: 1: 3.6, 3.5: 1: 3.8, 4: 1: 3.3, etc. Those skilled in the art can adjust the ratio of carbon dioxide extract (i.e., ganoderma lucidum spore oil), ethanol extract: and the content of the water extract is reasonably adjusted. Moreover, those skilled in the art will understand that, in the preparation of the polysaccharide-rich or triterpene-rich wall-removed product series, the weight ratio of the carbon dioxide extract (i.e., ganoderma spore oil) to the ethanol extract to the water extract (weight ratio) of the active ingredients embedded in the shell of the pellet is not limited to the above, and may be 3.6: 1: 12, 1: 2.5: 1, etc., and those skilled in the art may appropriately adjust the above weight ratio according to the actual product requirements.
In summary, the present invention provides the following technical solutions:
1. a wall-removed pellet containing Ganoderma spore powder comprises carbon dioxide extract (Ganoderma spore oil), ethanol extract and water extract of Ganoderma spore powder embedded in pellet shell, wherein the weight ratio of carbon dioxide extract, ethanol extract and water extract is 3-4: 1: 3-4.
2. The whole ganoderma lucidum spore powder de-walling pellet of item 1, which is prepared by a method comprising the steps of: :
(1) extracting Ganoderma spore powder with food-grade liquid carbon dioxide at 25-45 deg.C and 25-35MPa, collecting the obtained carbon dioxide extract which is spore oil, and separating to obtain residue 1;
(2) extracting the residue 1 with 1-15 times of 95% ethanol, 75% ethanol, and 50% ethanol at 60 deg.C for 1-5 hr, collecting ethanol extract, and separating to obtain residue 2;
(3) extracting the residue 2 with 1-20 times of hot water at 100 deg.C for 1-4 hr, and collecting to obtain hot water extract;
(4) mixing the extraction product and the extract obtained in the steps (1) - (3), mixing with 0.5-5 wt% of sodium alginate aqueous solution with the viscosity of 20-800cps, dripping into 0.5-5 wt% of calcium chloride aqueous solution while stirring to form spherical pellets, soaking the formed spherical pellets in 0.5-5 wt% of calcium chloride aqueous solution for 1-240 minutes, taking out, cleaning in distilled water, and drying to obtain the wall-removed full ganoderma spore powder pellets.
3. The whole ganoderma lucidum spore powder wall-removing pellet of claim 2, wherein in the step (4), the weight ratio of the combined product mixture of the steps (1) to (3) to the sodium alginate aqueous solution is 1:1 to 1: 10.
4. The total ganoderma spore powder wall-removing pellet of claim 2, wherein in the step (4), the weight ratio of the combined extraction products of the steps (1) to (3) to the sodium alginate aqueous solution is 1:1.5, 1:2, 1:3 or 1: 10.
5. The whole ganoderma lucidum spore powder wall-removed pellet of claim 2, wherein the viscosity of the sodium alginate used in step (4) is 200, 400 or 600cps at room temperature.
6. The whole ganoderma lucidum spore powder wall-removing pellet of claim 2, wherein the concentration of the sodium alginate aqueous solution used in the step (4) is 0.5% by weight or 1% by weight.
7. The whole ganoderma lucidum spore powder wall-removing pellet of claim 2, wherein the viscosity of the sodium alginate used in the step (4) is 200cps, and the concentration of the aqueous solution of the sodium alginate is 0.5 or 1 wt%.
8. The whole ganoderma lucidum spore powder wall-removing pellet of claim 2, wherein the viscosity of the sodium alginate used in the step (4) is 400cps, and the concentration of the sodium alginate aqueous solution used is 0.5 wt%.
9. The whole ganoderma lucidum spore powder wall-removing pellet of claim 2, wherein the viscosity of the sodium alginate used in the step (4) is 600cps, and the concentration of the sodium alginate aqueous solution used is 1% by weight.
10. The whole ganoderma spore powder de-walling pellet of item 2, wherein the concentration of the aqueous calcium chloride solution used in step (4) is 1 wt%, 2 wt%, 3 wt%, or 4 wt%, and the time for soaking the spherical pellet in the aqueous calcium chloride solution is 30 minutes, 60 minutes, 120 minutes, or 200 minutes.
11. The total ganoderma spore powder wall-removing pellet according to the item 2, which is spherical or nearly spherical, and has a diameter of 2.9-3.3 mm.
12. The whole ganoderma lucidum spore powder wall-removed pellet of claim 2, which remains in the original state in gastric juice and swells in intestinal juice for 2-3 hours until disintegration.
13. The total ganoderma lucidum spore powder wall-removing pellet of claim 2, wherein the spore powder utilization rate is more than 95%.
14. The total ganoderma spore powder wall-removed pellet of claim 2, wherein the weight ratio of the carbon dioxide extract (namely ganoderma spore oil) to the ethanol extract to the water extract in the active ingredients embedded in the pellet shell is 3.6: 1: 3.6.
15. The total ganoderma spore powder wall-removed pellet of claim 2, wherein the weight ratio of the carbon dioxide extract (namely ganoderma spore oil) to the ethanol extract to the water extract in the active ingredients embedded in the pellet shell is 3.5: 1: 3.8.
16. The total ganoderma spore powder wall-removed pellet of claim 2, wherein the weight ratio of the carbon dioxide extract (namely ganoderma spore oil) to the ethanol extract to the water extract in the active ingredients embedded in the pellet shell is 4: 1: 3.3.
The invention has the beneficial effects that:
1. the method provided by the invention realizes the wall removal of the spore powder in the real sense, completely retains all functional substances in the spore powder and concentrates the functional substances in one dosage form, and discards useless spore walls. The proportion of the effective substances is improved from about 50 percent to more than 95 percent (containing trace calcium alginate), thus solving the problem of low utilization rate of the effective substances of the common spore powder;
2. on the aspect of equivalent utilization of spore powder, the effect of taking 2g of spore powder can be achieved by taking about 1g of the wall-removing pellet, and the dosage is halved;
3. the ganoderma lucidum spore oil is embedded in the pellet, so that the problem of oxidative deterioration caused by exosmosis of the spore oil in the common wall-broken spore powder is solved;
4. the prepared pellet has good physical toughness and good fluidity, and solves the problems of sticky materials and difficult packaging caused by the seepage of spore oil of the wall-broken spore powder;
5. the micro-pill is easy to swallow, and solves the problem of poor taste caused by oral powder;
6. the prepared pellet has strong carrying capacity on active substances from spore powder, is stable in simulated artificial gastric juice and can be disintegrated and released in intestinal juice, and the problems of gastric irritation and gastric juice decomposition of common wall-broken spore powder are solved.
Except for reducing the original proportion of the effective components of the spore powder, the reinforced ganoderma lucidum spore powder wall-removing pellet preparation rich in polysaccharide, triterpene and the like can be prepared by adjusting the proportion of each extract.
Drawings
The above features and advantages of the present invention will become more apparent from the following detailed description when taken in conjunction with the accompanying drawings, in which:
FIG. 1 shows photographs of the de-wall pellets prepared in example 2 of the present invention swollen for 3 hours in 0.1mol/L hydrochloric acid solution (HCl, pH1.0) (A) simulating gastric juice and phosphate buffered saline (PBS, pH7.4) (B) simulating intestinal juice.
FIG. 2 shows photographs of the de-wall pellets prepared in example 2 of the present invention swollen for 12 hours in 0.1mol/L hydrochloric acid solution (HCl, pH1.0) (A) simulating gastric juice and phosphate buffered saline (PBS, pH7.4) (B) simulating intestinal juice.
FIG. 3 shows the swelling ratio curves (ratio of the outer diameter of the swollen microspheres to the outer diameter of the dried microspheres before swelling, 100%) of the de-wall micropellets prepared in example 2 of the present invention in different media.
Detailed Description
The invention is further described below with reference to specific examples, but it will be understood by those skilled in the art that the invention is not limited to these specific examples.
Example 1 preparation of Ganoderma spore powder extract and spore oil
The ganoderma lucidum spore powder extract and the spore oil used in the invention can be prepared according to the conventional method in the field, and the spore oil with the extraction rate of more than 15-20%, the ethanol extract with the extraction rate of more than 5% and the water extract with the extraction rate of more than 15-20% are generally selected for the invention. The "alcoholic extract" of spore powder generally refers to an alcoholic extract of spore powder, if not otherwise specified.
In addition, the inventor finds that the spore oil, the spore powder alcohol extract or the spore powder water extract with higher extraction rate can be obtained by the following preparation method:
the preparation method of the spore oil (namely, the method for extracting the spore powder by using liquid carbon dioxide) comprises the following steps:
1. putting the wall-broken ganoderma lucidum spore powder into an extraction kettle;
2. pumping liquid carbon dioxide, keeping the temperature of the extraction kettle at 40 ℃, and extracting under the pressure of 28 MPa;
3. adjusting the temperature of the separation chamber 1 to 40 ℃ and the pressure to 8MPa, and the temperature of the separation chamber 2 to 40 ℃ and the pressure to 5 MPa;
4. extracting for 3.5 hours, collecting extracted spore oil, and separating residue 1.
The preparation method of the spore powder ethanol extract comprises the following steps:
1. putting the residual wall-broken ganoderma lucidum spore powder residue 1 after extracting the spore oil by the liquid carbon dioxide into an extraction container;
2. adding 10 times of 95% ethanol, extracting at 60 deg.C for 2 hr, and filtering;
3. extracting the residue with 10 times of 75% ethanol at 60 deg.C for 2 hr, and filtering;
4. extracting the residue with 10 times of 50% ethanol at 60 deg.C for 2 hr, and filtering;
5. mixing the filtrates, concentrating, drying, pulverizing to obtain spore powder ethanol extract, and separating residue 2.
The preparation method of the spore powder hot water extract comprises the following steps:
1. putting the wall-broken spore powder residue 2 after extracting the spore powder by the ethanol into an extraction container;
2. adding 10 times of distilled water, extracting at 100 deg.C for 2 hr, and filtering;
3. extracting the residue with 10 times of distilled water at 100 deg.C for 2 hr, and filtering;
4. the filtrates were combined 2 times, concentrated, dried, and pulverized to obtain a hot water extract of spore powder (also referred to as "spore powder aqueous extract" in the present invention).
Mixing all the extracts prepared by the three extraction methods uniformly, or mixing Ganoderma spore oil, ethanol extract and Ganoderma spore powder water extract according to the natural ratio of Ganoderma spore oil to Ganoderma spore powder, i.e. 3-4: 1: 3-4 (weight ratio) to obtain the total effective components contained in the spore powder, which are referred to as "total Ganoderma spore powder extract", and the residue after hot water extraction is spore powder wall.
The product obtained by extracting spore powder with liquid carbon dioxide is called spore oil, the product obtained by extracting the residue after liquid carbon dioxide extraction with ethanol is called spore powder ethanol extract, and the product obtained by extracting the residue after ethanol extraction with hot water is called spore powder hot water extract (also called spore powder water extract). To distinguish from spore oil, a mixture of an ethanol extract of spore powder and an aqueous extract of spore powder is collectively referred to as spore powder extract. And the mixture obtained by combining the spore oil, the ethanol extract of the spore powder and the water extract of the spore powder is called as the 'total ganoderma spore powder extract'.
Example 2 pellet preparation example 1
Taking 4.4g of spore oil, 1.2g of ethanol extract and 4.4g of water extract prepared according to the method of example 1, namely 10g of total ganoderma spore powder extract, wherein the weight ratio of the spore oil to the ethanol extract to the water extract is about 3.6: 1: 3.6, mixing the mixture with 20g of sodium alginate solution (sodium alginate with the viscosity of 200cps purchased from the moon sea algae group) with the concentration of 0.5 weight percent and the viscosity of 200cps (room temperature), uniformly stirring the mixture, slowly dripping the mixture into calcium chloride solution with the concentration of 1 weight percent in a liquid drop manner while stirring when bubbles dissipate, soaking the mixture for 30 minutes, taking out the pellets, washing the pellets by using distilled water, and drying the pellets to obtain finished pellets.
The prepared pellet is spherical and nearly spherical, the diameter is 3.0-3.2mm, and the weight is 18.5-19.0 mg.
The whole preparation process needs to be aseptic, and the used water, sodium alginate solution and calcium chloride solution all need to be aseptic.
Example 3 pellet preparation example 2
Taking 4.2g of spore oil, 1.2g of ethanol extract and 4.6g of water extract prepared according to the method of example 1, namely 10g of total ganoderma spore powder extract, wherein the weight ratio of the spore oil to the ethanol extract to the water extract is about 3.5: 1: 3.8, mixing the mixture with 15g of sodium alginate solution (sodium alginate with the viscosity of 400cps purchased from a moon sea algae group) with the concentration of 0.5 weight percent and the viscosity of 400cps (room temperature), stirring uniformly, slowly dropping the mixture into a calcium chloride solution with the concentration of 3 weight percent in a liquid drop manner while stirring until bubbles dissipate, soaking for 30 minutes, taking out the pellets, washing with distilled water, and drying to obtain finished pellets. .
The prepared pellet is spherical and nearly spherical, the diameter is 2.9-3.0mm, and the weight is 17.8-18.5 mg.
The whole preparation process needs to be aseptic, and the used water, sodium alginate solution and calcium chloride solution all need to be aseptic.
Example 4 pellet preparation example 3
Taking 4.8g of spore oil, 1.2g of ethanol extract and 4.0g of water extract prepared according to the method of example 1, namely 10g of total ganoderma spore powder extract, wherein the weight ratio of the spore oil to the ethanol extract to the water extract is about 4: 1: 3.3, mixing the spore oil to the ethanol extract to the water extract with 30g of sodium alginate solution (sodium alginate with the viscosity of 600cps is purchased from the Mingyuehai algae group) with the concentration of 1 weight percent and the viscosity of 600cps (room temperature), uniformly stirring, slowly dropping the mixture into a calcium chloride solution with the concentration of 2 weight percent in a liquid drop manner while stirring when bubbles dissipate, taking out the pellets after soaking for 60 minutes, washing the pellets with distilled water and drying to obtain finished pellets.
The prepared pellet is spherical and nearly spherical, the diameter is 3.1-3.3mm, and the weight is 21.0-21.5 mg.
The whole preparation process needs to be aseptic, and the used water, sodium alginate solution and calcium chloride solution all need to be aseptic.
In the above examples 2-4, the ratio of the spore powder extracts in the spore powder is determined according to the natural ratio, the prepared pellet represents all the functional substances of the spore powder after shelling, and if the pellet for enhancing polysaccharide or triterpene needs to be prepared, the pellet can be prepared by adjusting the ratio, specifically, the following examples are included:
example 5 pellet preparation example 4
Polysaccharide-enriched spore powder wall-removing pellet: taking 4.4g of spore oil, 1.2g of ethanol extract and 4.4g of water extract, namely 10g of total ganoderma spore powder extract, wherein the weight ratio of the spore oil to the ethanol extract to the water extract is about 3.6: 1: 3.6, adding 10g of spore powder water extract (which is prepared by the method of the embodiment 1, wherein the weight ratio of the spore oil to the ethanol extract to the water extract is about 3.6: 1: 12), mixing with 60g of sodium alginate solution (sodium alginate with the viscosity of 200cps is purchased from the Minghai seaweed group) with the concentration of 1 weight percent and the viscosity of 200cps (room temperature), stirring uniformly, after bubbles dissipate, slowly dripping into calcium chloride solution with the concentration of 4 weight percent in a liquid drop manner while stirring, soaking for 120 minutes, taking out the pellets, washing with distilled water and drying to obtain finished pellets.
The prepared pellet is spherical and nearly spherical, the diameter is 3.2-3.3mm, and the weight is 22.5-23.0 mg.
The whole preparation process needs to be aseptic, and the used water, sodium alginate solution and calcium chloride solution all need to be aseptic.
Example 6 pellet preparation example 5
Spore powder wall-removing pellet for reinforcing triterpene: taking 4.4g of spore oil, 1.2g of ethanol extract and 4.4g of water extract, namely 10g of total ganoderma spore powder extract, wherein the weight ratio of the spore oil to the ethanol extract to the water extract is about 3.6: 1: 3.6, adding 10g of spore powder ethanol extract (which are prepared by the method of the embodiment 1, wherein the weight ratio of the spore oil to the ethanol extract to the water extract is about 1: 2.5: 1), mixing with 200g of sodium alginate solution (sodium alginate with the viscosity of 200cps is purchased from the Mingyuehai algae group) with the concentration of 1 weight percent and the viscosity of 200cps (room temperature), stirring uniformly, after bubbles dissipate, slowly dripping into calcium chloride solution with the concentration of 1 weight percent in a liquid drop manner while stirring, soaking for 200 minutes, taking out the pellets, washing with distilled water and drying to obtain finished pellets.
The prepared pellet is spherical and nearly spherical, the diameter is 3.2-3.3mm, and the weight is 22.5-23.0 mg.
The whole preparation process needs to be aseptic, and the used water, sodium alginate solution and calcium chloride solution all need to be aseptic.
Example 7 comparison of Dewalled micropellets prepared in accordance with the invention with spore powder, a conventional "Dewalled" product
The de-walled pellets prepared in example 2 were compared to spore powder, a common "de-walled" product currently known in the art.
The ordinary "wall-removed" products refer to related products currently developed in the art using only aqueous extracts of ganoderma lucidum spore powder, without any ganoderma lucidum spore oil and any alcohol extracts of ganoderma lucidum spore powder, such as being packaged in sachets or filled into capsules.
TABLE 1 sensory comparison of the Dewalled pellets prepared according to the invention with spore powder, a conventional "Dewalled" product
As can be seen from table 1, the wall-removed pellet prepared by the present invention has comprehensive sensory characteristics of good fluidity, convenient filling, convenient administration, and good palatability, compared with common wall-removed and common wall-broken spore powder products.
TABLE 2 comparison of the utilization of the inventive de-walled pellets with spore powder, a common "de-walled" product
As can be seen from Table 2, although the nutrient components in the spore powder can be completely absorbed by taking the common spore powder, the wall-broken spore powder only utilizes about 50-60% of the effective substances because the wall-broken spore powder contains 40-50% of useless spore walls; the nature of the common 'wall-removing' product is a hot water extract of ganoderma lucidum spore powder, which represents that polysaccharide is taken as a main effective component and does not contain spore oil and alcohol extract, so that only 15-20% of effective components in the spore powder are utilized; the wall-removing pellet prepared by the invention contains all effective components in spore powder, the product does not contain any spore wall, the utilization rate of the spore powder is up to more than 95% (the part with extraction loss and trace calcium alginate are deducted), and the utilization rate is greatly improved.
In addition, the de-wall pellets prepared in example 2 of the present invention were swelled in 0.1mol/L hydrochloric acid solution (HCl, pH1.0) simulating gastric juice (FIGS. 1A and 2A) and phosphate buffered saline (PBS, pH7.4) simulating intestinal juice (FIGS. 1B and 2B), respectively, for 3 hours and 12 hours, and the corresponding swelling ratios (ratio of outer diameter of microspheres after swelling to outer diameter of dried microspheres before swelling, 100%) were plotted, and the results are shown in FIGS. 1, 2 and 3.
Fig. 1-3 illustrate that the pellet prepared by the invention keeps the original shape in gastric juice and swells in intestinal juice for 2-3 hours until disintegration, so that the effective components can be protected from being damaged by gastric acid and enter the intestinal tract for direct absorption.
It should be understood that while the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it will be understood by those of ordinary skill in the art that various changes in form and details may be made therein, and any combination of the various embodiments may be made therein without departing from the spirit and scope of the present invention as defined by the following claims.
Claims (10)
1. A total ganoderma spore powder wall-removing pellet comprises the active ingredients of a carbon dioxide extract, an ethanol extract and a water extract of ganoderma spore powder embedded in a pellet shell, wherein the weight ratio of the carbon dioxide extract to the ethanol extract to the water extract is 3-4: 1: 3-4,
wherein the total ganoderma lucidum spore powder wall-removing pellet is prepared by the method comprising the following steps:
(1) extracting Ganoderma spore powder with food-grade liquid carbon dioxide at 25-45 deg.C and 25-35MPa, collecting the obtained carbon dioxide extract which is spore oil, and separating to obtain residue 1;
(2) extracting the residue 1 with 1-15 times of 95% ethanol, 75% ethanol, and 50% ethanol at 60 deg.C for 1-5 hr, collecting ethanol extract, and separating to obtain residue 2;
(3) extracting the residue 2 with 1-20 times of hot water at 100 deg.C for 1-4 hr, and collecting to obtain hot water extract;
(4) mixing the extraction product and the extract obtained in the steps (1) - (3), mixing with 0.5-5 wt% of sodium alginate aqueous solution with the viscosity of 20-800cps, dripping into 0.5-5 wt% of calcium chloride aqueous solution while stirring to form spherical pellets, soaking the formed spherical pellets in 0.5-5 wt% of calcium chloride aqueous solution for 1-240 minutes, taking out, cleaning in distilled water, and drying to obtain the wall-removed whole ganoderma spore powder pellets.
2. The whole ganoderma lucidum spore powder wall-removing pellet as claimed in claim 1, wherein in the step (4), the weight ratio of the combined product mixture of the steps (1) to (3) to the sodium alginate aqueous solution is 1:1 to 1: 10.
3. the whole ganoderma lucidum spore powder wall-removing pellet of claim 1, wherein in the step (4), the weight ratio of the combined product mixture of the steps (1) to (3) to the sodium alginate aqueous solution is 1:1.5, 1:2, 1:3 or 1: 10.
4. The whole ganoderma lucidum spore powder wall-removing pellet of claim 1, wherein the viscosity of the sodium alginate used in step (4) is 200, 400 or 600cps at room temperature.
5. The whole ganoderma lucidum spore powder wall-removing pellet of claim 1, wherein the concentration of the sodium alginate aqueous solution used in step (4) is 0.5% by weight or 1% by weight.
6. The whole ganoderma lucidum spore powder wall-removing pellet of claim 1, wherein the viscosity of the sodium alginate used in step (4) is 200cps and the concentration of the aqueous sodium alginate solution used is 0.5 or 1 wt%.
7. The whole ganoderma lucidum spore powder wall-removing pellet of claim 1, wherein the viscosity of the sodium alginate used in step (4) is 400cps and the concentration of the aqueous sodium alginate solution used is 0.5 wt%.
8. The whole ganoderma lucidum spore powder wall-removing pellet of claim 1, wherein the viscosity of the sodium alginate used in step (4) is 600cps and the concentration of the aqueous sodium alginate solution used is 1% by weight.
9. The whole ganoderma spore powder de-walling pellet of claim 1, wherein the concentration of the aqueous calcium chloride solution used in step (4) is 1%, 2%, 3% or 4% by weight, and the time for soaking the spherical pellets in the aqueous calcium chloride solution is 30 minutes, 60 minutes, 120 minutes or 200 minutes.
10. The whole ganoderma lucidum spore powder wall-removing pellet of claim 1, which is spherical or nearly spherical and has a diameter of 2.9-3.3 mm.
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| 刘国健.灵芝孢子不同有效部位提取及体内抗肿瘤作用研究.《中国优秀硕士学位论文全文数据库医药卫生科技辑》.2018,E057-100. * |
| 灵芝孢子不同有效部位提取及体内抗肿瘤作用研究;刘国健;《中国优秀硕士学位论文全文数据库医药卫生科技辑》;20180228;E57-100 * |
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