CN112007057A - Preparation method of wall-broken ganoderma lucidum spore powder capsule and wall-broken ganoderma lucidum spore powder capsule - Google Patents
Preparation method of wall-broken ganoderma lucidum spore powder capsule and wall-broken ganoderma lucidum spore powder capsule Download PDFInfo
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- CN112007057A CN112007057A CN202010821424.XA CN202010821424A CN112007057A CN 112007057 A CN112007057 A CN 112007057A CN 202010821424 A CN202010821424 A CN 202010821424A CN 112007057 A CN112007057 A CN 112007057A
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- 206010028980 Neoplasm Diseases 0.000 description 1
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- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
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- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 1
- 235000019796 monopotassium phosphate Nutrition 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 1
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
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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
-
- 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
- A61K9/4808—Preparations in capsules, e.g. of gelatin, of chocolate characterised by the form of the capsule or the structure of the filling; Capsules containing small tablets; Capsules with outer layer for immediate drug release
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P35/00—Antineoplastic agents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P37/00—Drugs for immunological or allergic disorders
- A61P37/02—Immunomodulators
- A61P37/04—Immunostimulants
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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
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/13—Preparation or pretreatment of starting material involving cleaning, e.g. washing or peeling
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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
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/19—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles lyophilised, i.e. freeze-dried, solutions or dispersions
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Abstract
The application relates to the field of health-care medicinal preparations, and particularly discloses a preparation method of a wall-broken ganoderma lucidum spore powder capsule and the wall-broken ganoderma lucidum spore powder capsule. The preparation method of the capsule of the wall-broken ganoderma lucidum spore powder comprises the following steps: mixing 94-98% of wall-broken ganoderma lucidum spore powder and 2-6% of ganoderma lucidum fine powder according to the mass percentage, granulating, and freeze-drying to obtain freeze-dried granules with the water rate of less than 7%; and then filling the capsule to obtain the wall-broken ganoderma lucidum spore powder capsule. Wherein the wall-broken ganoderma lucidum spore powder is prepared by the working procedures of cleaning, soaking, filtering, freeze drying and wall breaking; the ganoderma lucidum fine powder is prepared by the processes of soaking, washing, extracting, concentrating, alcohol precipitating and drying. The content of the wall-broken ganoderma lucidum spore powder capsule prepared by the method has high contents of polysaccharide, spore oil and ergosterol, and simultaneously, the active ingredients have the advantage of being easily absorbed and utilized by human bodies. The application also correspondingly discloses a wall-broken ganoderma lucidum spore powder capsule which is prepared by the preparation method.
Description
Technical Field
The invention relates to the field of health-care medicinal preparations, in particular to a preparation method of a wall-broken ganoderma lucidum spore powder capsule and the wall-broken ganoderma lucidum spore powder capsule.
Background
Ganoderma lucidum is a traditional Chinese herbal medicine, the application history of which has been over 2000 years, and the Ganoderma lucidum used as the Chinese herbal medicine is mainly the dried fruiting body of Ganoderma lucidum (Ganoderma lucidum) or Ganoderma sinensis (Ganoderma sinense) of Polyporaceae. However, studies have shown that ganoderma lucidum extracts have the effect of enhancing immunity or directly inducing cancer cell death to exert anticancer activity. Ganoderma spore is the seed ejected after Ganoderma development, and is collected to be powder, and is called Ganoderma spore powder. The ganoderma lucidum spore powder has high polysaccharide content, and the polysaccharide is an effective component which is recognized at home and abroad and improves the immunologic function. The content of effective components of the ganoderma lucidum spores released when the ganoderma lucidum sporocarp is mature is 75 times higher than that of the ganoderma lucidum. The wall-broken ganoderma lucidum spore powder or ganoderma lucidum spore powder extract is a conventional raw material for preparing medicaments or functional health care products.
In the related art, the main purpose of improving the efficacy of ganoderma lucidum medicaments or health-care products is to improve the content of polysaccharide. For example, chinese patent application publication No. CN1377702A (published: 20021106) discloses a capsule of wall-broken ganoderma lucidum spore powder, which comprises raw materials of wall-broken ganoderma lucidum spore powder and refined ganoderma lucidum powder, wherein the refined ganoderma lucidum powder is prepared by crushing ganoderma lucidum fruiting bodies, extracting with water (2-4 hours × 2 times), sieving, concentrating, drying and pulverizing, and the polysaccharide content of the finally prepared capsule of wall-broken ganoderma lucidum spore powder meets the requirement of not less than 35 mg/g; CN101091727A discloses a method for preparing a capsule of wall-broken ganoderma lucidum spore powder, which uses wall-broken ganoderma lucidum spore powder and spore powder as raw materials for preparing the capsule by extracting (three times of water extraction and then further alcohol extraction) to obtain an extract, so that the content of polysaccharide in each 100g of capsule filling material reaches 5.84-6.12 g.
Meanwhile, researches show that in the bioactive components of the ganoderma, except polysaccharides, sterol active substances also have the effects of improving immunity and inhibiting tumors, the ergosterol content in the sterol separated and extracted from the ganoderma is the highest, and the difference of the extraction method or the preparation method directly influences the effective yield of the ergosterol. The related art mentioned above, although the content of polysaccharide in the extract is increased to some extent, does not relate to how to increase the effective content of sterol active substance in the prepared ganoderma lucidum spore powder capsule.
Therefore, the existing preparation method of the spore powder microcapsule still has room for further improvement so as to improve the content of the sterol active ingredients while improving the content of the polysaccharide.
Disclosure of Invention
In order to improve the content of polysaccharide and the content of sterol active ingredients in the ganoderma lucidum spore powder capsule, the application provides a preparation method of a wall-broken ganoderma lucidum spore powder capsule and the wall-broken ganoderma lucidum spore powder capsule.
In a first aspect, the application provides a method for preparing a wall-broken ganoderma lucidum spore powder capsule, which adopts the following technical scheme:
a method for preparing wall-broken Ganoderma spore powder capsule comprises the following steps,
a material mixing step: mixing wall-broken Ganoderma spore powder 94-98% and Ganoderma fine powder 2-6% to obtain total mixed powder;
the wall-broken ganoderma lucidum spore powder is prepared by the following processes:
p1, cleaning the ganoderma lucidum spore powder with clear water to obtain cleaned spore powder; p2, soaking the cleaned spore powder in water, fully stirring again, and filtering to obtain filtrate containing Ganoderma spore powder; standing to allow the filtrate to naturally precipitate until layering, removing supernatant, and retaining the bottom layer spore powder mixture; p3, freeze-drying the spore powder mixture obtained in the step P2 to obtain freeze-dried spore powder, and controlling the water content of the freeze-dried spore powder to be less than 4%; p4, performing wall breaking treatment on the freeze-dried spore powder obtained in the step P3 by using a wall breaking machine to obtain wall-broken ganoderma lucidum spore powder for later use;
wherein the ganoderma lucidum fine powder is prepared by the following process:
s1, soaking the lucid ganoderma fruit bodies or the lucid ganoderma slices in water, washing with water, and draining to obtain the clean lucid ganoderma fruit bodies or the lucid ganoderma slices; s2, adding the cleaned Ganoderma encarpium or Ganoderma slice into water, heating, extracting at 100 deg.C for 0.8-1.2 hr, filtering and retaining the filtrate; extracting under the same conditions for 2 times, mixing filtrates, and concentrating to obtain concentrated filtrate; s3, mixing the concentrated filtrate according to the mass ratio of 1: (2.0-3.0) adding ethanol with the concentration more than or equal to 80% for alcohol precipitation, standing and layering; s4, removing the supernatant liquid of the alcohol precipitation in the step S3, reserving the precipitate, and drying to obtain the ganoderma lucidum fine powder for later use;
a granulation step: granulating the total mixed powder, and freeze-drying to obtain freeze-dried granules, wherein the water content of the freeze-dried granules is controlled to be less than 7%;
and (3) filling capsules: and (4) filling the freeze-dried granules obtained in the granulation step into capsules to obtain the wall-broken ganoderma lucidum spore powder capsules.
Through adopting above-mentioned technical scheme, compare in correlation technique, the broken wall glossy ganoderma spore powder as the raw materials in this application needs to wash in proper order, filter, freeze-drying and broken wall processing according to specific process flow and obtains, the secondary freeze-drying of the granulation step of deuterogamying makes glossy ganoderma spore powder active ingredient precipitate more easily, and reduced the loss of active ingredient in the processing procedure raw materials by a wide margin, still assist the glossy ganoderma essence powder that specific technology of specific dosage was drawed in the preparation technology of this application, the broken wall glossy ganoderma spore powder capsule that finally makes has higher polysaccharide, spore oil and ergosterol content, especially ergosterol content promotes most notably. Meanwhile, the ganoderma lucidum bioactive components in the capsule of the wall-broken ganoderma lucidum spore powder prepared by the method are easier to be absorbed by human bodies, and the effective utilization rate of the active components is improved.
Preferably, the freeze-drying process of the P3 step is as follows:
firstly, under the condition of 0.8MPa of vacuum degree, the temperature is reduced to minus 42 to minus 38 ℃ at the speed of 0.4 to 0.6 ℃/min, and the temperature is preserved for 1.8 to 2.2 hours; then, under the condition of the vacuum degree of 1.0MPa, the temperature is increased to 38-42 ℃ at the speed of 0.1-0.15 ℃/min, and the temperature is preserved for 9-11 hours.
By adopting the technical scheme, the separation of active ingredients of the ganoderma lucidum is better facilitated, the loss of the active ingredients in the processing process is reduced, and the content effects of the polysaccharide, the spore oil and the ergosterol in the wall-broken ganoderma lucidum spore powder capsule are improved remarkably.
Preferably, the freeze-drying process in the granulation step is as follows:
firstly, under the condition of 0.8MPa of vacuum degree, the temperature is reduced to minus 42 to minus 38 ℃ at the speed of 0.4 to 0.6 ℃/min, and the temperature is preserved for 1.8 to 2.2 hours; then, under the condition of the vacuum degree of 1.0MPa, the temperature is increased to 38-42 ℃ at the speed of 0.1-0.15 ℃/min, and the temperature is preserved for 9-11 hours.
By adopting the technical scheme, the secondary freeze drying can further promote the active ingredients to be separated out, simultaneously reduce the ineffective loss of the active ingredients, and has obvious effects of improving the content of polysaccharide, spore oil and ergosterol in the wall-broken ganoderma lucidum spore powder capsule.
Preferably, the specific operation steps of the P1 step are as follows:
adding clear water into the ganoderma lucidum spore powder according to the proportion that 70-80 parts by weight of clear water is added into every 3 parts by weight of ganoderma lucidum spore powder, stirring to fully disperse the ganoderma lucidum spore powder, and naturally precipitating for 1.0-2.0 hours; after precipitation, removing the upper clear water and reserving the bottom precipitation mixture; repeating the operation for 4-6 times until no suspended matters exist in the upper clear water, and obtaining the cleaned spore powder.
Through adopting above-mentioned technical scheme, can effectively clear away glossy ganoderma spore on the one hand and smuggle secretly or adnexed impurity, on the other hand so handle and can make glossy ganoderma spore powder fully absorb water and swell, cooperate follow-up freeze drying and broken wall processing again for glossy ganoderma active ingredient can fully separate out, does benefit to the active ingredient content in the promotion broken wall glossy ganoderma spore powder capsule.
Preferably, in the P2 step:
adding the cleaned spore powder into 70-80 parts of clear water, soaking for 1.0-2.0 hours, fully stirring again, and filtering.
By adopting the technical scheme, the ganoderma lucidum spores are further enabled to absorb water and swell, and subsequent freeze drying and wall breaking are facilitated.
Preferably, in the P2 step:
adopts double-layer filter screens for filtration, the mesh number of the first layer filter screen is 90-110 meshes, and the mesh number of the second layer filter screen is 190-210 meshes.
By adopting the technical scheme, the impurity removal effect is good, and the quality stability of the wall-broken ganoderma lucidum spore powder capsule product are favorably improved.
Preferably, in the P4 step:
and (3) the temperature of circulating cooling water of the wall breaking machine is less than 22 ℃, the feeding amount is 1.8-2.2 kg each time, and the obtained wall-broken ganoderma lucidum spore powder is vacuum-packaged for later use.
By adopting the technical scheme, the wall breaking rate of the ganoderma lucidum spore powder can reach more than 95%, meanwhile, the damage of high temperature generated by friction in the wall breaking process to the active ingredients of the ganoderma lucidum is reduced, and the content of the active ingredients in the wall-broken ganoderma lucidum spore powder capsule is favorably improved.
Preferably, in the step S1:
soaking Ganoderma fruiting body or Ganoderma slice in water for 20-30min, wherein the water is added in an amount of 20-25 weight parts per 1 weight part of Ganoderma fruiting body or Ganoderma slice.
By adopting the technical scheme, the active ingredients in the ganoderma lucidum can be fully extracted, the subsequent concentration time is favorably shortened, and the damage of the active ingredients in the concentration process is favorably reduced (the loss of the active ingredients such as polysaccharide, spore oil, ergosterol and the like is easily increased by long-time high-temperature treatment).
Preferably, in the step S2:
adding cleaned Ganoderma encarpium or Ganoderma slice into 13-17 weight parts of water, heating and extracting, filtering, and retaining filtrate; repeatedly extracting for 2-5 times under the same conditions, combining the filtrates, and concentrating to obtain the final product with Baume degree of 1.0-1.4.
By adopting the technical scheme, compared with the conventional technology of preparing the wall-broken ganoderma lucidum spore powder capsule by taking the spore powder with high active ingredient content as the raw material, the method directly takes the ganoderma lucidum fruiting body or the ganoderma lucidum slice as the raw material to prepare the ganoderma lucidum fine powder, and reduces the preparation cost of the wall-broken ganoderma lucidum spore powder capsule to a certain extent; on the other hand, the finally prepared capsule of the wall-broken ganoderma lucidum spore powder still keeps higher content of active effective components by combining multiple extraction and concentration means and matching adjustment of the material ratio of the capsule of the wall-broken ganoderma lucidum spore powder and optimization of the preparation process.
In a second aspect, the application provides a ganoderma lucidum spore powder capsule, which adopts the following technical scheme:
a capsule of wall-broken Ganoderma spore powder is prepared by any one of the above preparation methods.
In conclusion, the invention has the following beneficial effects:
1. according to the method, the wall-broken ganoderma lucidum spore powder prepared by a specific process and the ganoderma lucidum fine powder prepared by the specific process are selected as raw materials, are mixed according to a specific proportion, and are subjected to granulation, freeze drying and capsule filling to obtain the wall-broken ganoderma lucidum spore powder capsule, so that the content of active ingredients (polysaccharide, spore oil and ergosterol) in the wall-broken ganoderma lucidum spore powder capsule is improved, and meanwhile, experiments show that the active ingredients in the wall-broken ganoderma lucidum spore powder capsule prepared by the method are easier to absorb.
2. In the preferred scheme, freeze drying is carried out according to a specific process, and the content of active ingredients in the prepared capsule of the wall-broken ganoderma lucidum spore powder is obviously improved.
3. The ganoderma lucidum fine powder is prepared by extracting ganoderma lucidum sporocarp or ganoderma lucidum slices serving as raw materials through a special process, and the preparation cost of the capsule of the wall-broken ganoderma lucidum spore powder is reduced.
4. The application also correspondingly discloses a wall-broken ganoderma lucidum spore powder capsule which is prepared by the preparation method of the wall-broken ganoderma lucidum spore powder capsule and has the advantages of high content of active ingredients and easier absorption of the active ingredients.
Detailed Description
Preparation example of wall-broken Ganoderma spore powder
Preparation example A
A preparation process of wall-broken ganoderma lucidum spore powder comprises the following steps:
p1, adding fresh water into the ganoderma spore powder according to the proportion that each 3 kg of ganoderma spore powder is added with 75 kg of fresh water, stirring to fully disperse the ganoderma spore powder, and naturally precipitating for 1.5 h; after precipitation, removing the upper clear water and reserving the bottom precipitation mixture; repeating the cleaning operation for 5 times until no suspended matter exists in the upper clear water, and obtaining cleaned spore powder;
p2, adding the cleaned spore powder into 75 kg of clean water, soaking for 1.5h, fully stirring again, filtering by adopting a double-layer filter screen, wherein the mesh number of the first layer of filter screen is 100 meshes, the mesh number of the second layer of filter screen is 200 meshes, and keeping the filtrate containing the ganoderma spore powder; standing to allow the filtrate to naturally precipitate until layering, removing supernatant, and retaining the bottom layer spore powder mixture;
p3, cooling the spore powder mixture obtained in the step P2 to-25 ℃ at the speed of 3.8 ℃/min under the condition that the vacuum degree is 0.8MPa, and preserving the heat for 2.0 hours; then, under the condition that the vacuum degree is 1.0MPa, the temperature is increased to 23 ℃ at the speed of 10.5 ℃/min, and the temperature is kept for 10 hours, so that freeze-dried spore powder is obtained, and the water content of the freeze-dried spore powder is controlled to be less than 4 percent;
and P4, performing wall breaking treatment on the freeze-dried spore powder obtained in the step P3 by using a wall breaking machine, wherein the circulating cooling water temperature of the wall breaking machine is 22 ℃, the feeding amount of the wall breaking machine is 2.0 kg each time, so that wall-broken ganoderma lucidum spore powder with the wall breaking rate of more than or equal to 95% is obtained, and vacuum-packaging the wall-broken ganoderma lucidum spore powder for later use by using an aluminum-plastic composite bag.
Preparation examples B to D
Preparation examples B-D all relate to a preparation process of wall-broken ganoderma lucidum spore powder, and the process steps are basically the same, and the difference is only that the process parameters are different.
The process comprises the following steps:
p1, adding clean water into the ganoderma lucidum spore powder according to the proportion that 70-80 kg of water are added into every 3 kg of ganoderma lucidum spore powder, stirring to ensure that the ganoderma lucidum spore powder is fully dispersed, and naturally precipitating for 1.0-2.0 hours; after precipitation, removing the upper clear water and reserving the bottom precipitation mixture; repeating the operation for 4-6 times until no suspended matter exists in the upper clear water, and obtaining the cleaned spore powder;
p2, adding the cleaned spore powder into 70-80 kg of clean water, soaking for 1.0-2.0 hours, then fully stirring again, filtering, and filtering by adopting a double-layer filter screen, wherein the mesh number of the first layer of filter screen is 90-110 meshes, the mesh number of the second layer of filter screen is 190-210 meshes, and keeping the filtrate containing the ganoderma lucidum spore powder; standing to allow the filtrate to naturally precipitate until layering, removing supernatant, and retaining the bottom layer spore powder mixture;
p3, cooling the spore powder mixture obtained in the step P2 to-42 to-38 ℃ at the speed of 0.4 to 0.6 ℃/min under the condition that the vacuum degree is 0.8MPa, and preserving the heat for 1.8 to 2.2 hours; then, under the condition of the vacuum degree of 1.0MPa, heating to 38-42 ℃ at the speed of 0.1-0.15 ℃/min, and preserving the heat for 9-11 hours to obtain freeze-dried spore powder, wherein the water content of the freeze-dried spore powder is controlled to be less than 4 percent;
and P4, performing wall breaking treatment on the freeze-dried spore powder obtained in the step P3 by using a wall breaking machine, wherein the circulating cooling water temperature of the wall breaking machine is less than 22 ℃, the feeding amount is 1.8-2.2 kg each time, and the wall-broken ganoderma lucidum spore powder with the wall breaking rate of more than or equal to 95% is obtained and is subjected to vacuum packaging by using an aluminum-plastic composite bag for later use.
The process parameters of the individual process steps of preparation examples B to D are specified in Table 1.
TABLE 1 preparation examples A-D Process parameter Table
The Ganoderma spore powder selected in preparation examples A-D is spore powder of Ganoderma lucidum in Taishan mountain, and Ganoderma spore powder of other production places can be selected in other preparation examples.
Preparation example of Ganoderma lucidum Fine powder
Preparation example a
A preparation process of Ganoderma fine powder comprises the following steps:
s1, taking the ganoderma lucidum slices, adding 22.5 kg of water to 1 kg of ganoderma lucidum slices, soaking for 25min, washing with water, and draining to obtain cleaned ganoderma lucidum slices;
s2, adding the cleaned ganoderma lucidum slices into 15 kg of water, heating, extracting at 100 ℃ for 1.0 hour, filtering, keeping filtrate, and concentrating the filtrate until the Baume degree is 1.2;
s3, mixing the concentrated filtrate according to the mass ratio of 1: 2.5, adding 80 percent ethanol according to the proportion to carry out alcohol precipitation, standing and layering;
s4, removing the supernatant liquid after the alcohol precipitation in the step S3, reserving the precipitate, and drying in vacuum to obtain the ganoderma lucidum fine powder for later use.
Preparation examples b to d
The preparation examples b-d all relate to a preparation process of ganoderma lucidum fine powder, the process steps are basically the same, and the difference is only that the process parameters of each step are different.
The process comprises the following steps:
s1, soaking the ganoderma lucidum slices in water for 20-30min, wherein the water adding amount is 20-25 kg of water for each 1 kg of ganoderma lucidum slices, washing with water, and draining to obtain cleaned ganoderma lucidum slices;
s2, adding the cleaned ganoderma lucidum slices into 13-17 kg of water, heating, extracting at 100 ℃ for 0.8-1.2 hours, and filtering to keep filtrate; repeatedly extracting for 2-5 times under the same conditions, combining the filtrates, and concentrating to obtain a concentration end point with a Baume degree of 1.0-1.4;
s3, mixing the concentrated filtrate according to the mass ratio of 1: (2.0-3.0) adding ethanol with the concentration more than or equal to 80% for alcohol precipitation, standing for 24h for layering;
s4, removing the supernatant liquid after the alcohol precipitation in the step S3, reserving the precipitate, and drying to obtain the ganoderma lucidum fine powder for later use.
The process parameters of the individual process steps of preparation examples b to d are specified in Table 2.
TABLE 2 Process parameter Table of preparation examples a-d
The ganoderma lucidum slices in the preparation examples a-d are Taishan ganoderma lucidum slices meeting the requirements of Chinese pharmacopoeia (2015 edition), and ganoderma lucidum slices or ganoderma lucidum fruiting bodies in other production places can be selected as preparation raw materials of ganoderma lucidum fine powder in other preparation examples.
Examples
Examples 1 to 3
Embodiments 1-3 all relate to a method for preparing a capsule of wall-broken ganoderma lucidum spore powder, which comprises the following steps:
(I) a material mixing step
Weighing 94-98% of wall-broken ganoderma lucidum spore powder and 2-6% of ganoderma lucidum fine powder by mass percent, and putting the wall-broken ganoderma lucidum spore powder and the ganoderma lucidum fine powder into a mixer to mix for more than 30min to obtain the total mixed powder which is uniformly mixed.
Wherein, the wall-broken ganoderma lucidum spore powder is prepared by the preparation example A, the ganoderma lucidum fine powder is prepared by the preparation example b, and the mixture ratio of the total mixed materials in the examples 1-3 is shown in the table 3.
TABLE 3 raw material ratio table of total mixed powder in examples 1-3
| Components | Example 1 | Example 2 | Example 3 |
| Wall-broken ganoderma lucidum spore powder | 94wt％ | 96wt％ | 98wt％ |
| Ganoderma lucidum fine powder | 6wt％ | 4wt％ | 2wt％ |
(II) a granulation step
And (3) granulating the total mixed powder, and freeze-drying to obtain freeze-dried granules, wherein the water content of the freeze-dried granules is controlled to be less than 7%.
The freeze drying process comprises the following steps:
firstly, under the condition of 0.8MPa of vacuum degree, the temperature is reduced to-25 ℃ at the speed of 3.8 ℃/min, and the temperature is kept for 2.0 hours; then, under the condition of the vacuum degree of 1.0MPa, the temperature is increased to 23 ℃ at the speed of 10.5 ℃/min, and the temperature is preserved for 10 hours, so that the water content in the material particles is reduced to below 7 percent.
(III) Capsule filling
And (3) filling the freeze-dried granules obtained in the granulation step into capsules, wherein each capsule is filled with 0.25g, and the allowable deviation is +/-9%, so that the wall-broken ganoderma lucidum spore powder capsules are obtained.
Examples 4 to 6
Embodiments 4 to 6 all relate to a method for preparing a capsule of wall-broken ganoderma lucidum spore powder, all based on embodiment 2, and are different from embodiment 2 only in the freeze-drying process of the granulation step, and the specific freeze-drying process is as follows:
firstly, under the condition of 0.8MPa of vacuum degree, the temperature is reduced to minus 42 to minus 38 ℃ at the speed of 0.4 to 0.6 ℃/min, and the temperature is preserved for 1.8 to 2.2 hours; then, under the condition of the vacuum degree of 1.0MPa, the temperature is increased to 38-42 ℃ at the speed of 0.1-0.15 ℃/min, and the temperature is preserved for 9-11 hours, so that the water content of the material particles is reduced to below 7 percent.
The process parameters of the freeze-drying procedure for the granulation steps of examples 4-6 are detailed in figure 4.
TABLE 4 table of the freeze-drying process parameters for the granulation steps of examples 4-6
Examples 7 to 9
Embodiments 7 to 9 all relate to a method for preparing a capsule of wall-broken ganoderma lucidum spore powder, all based on embodiment 6, and are different from embodiment 6 only in that the wall-broken ganoderma lucidum spore powder in the step of mixing materials is prepared by different preparation methods, specifically:
the wall-broken ganoderma lucidum spore powder of example 7 is prepared by the preparation example B;
the wall-broken ganoderma lucidum spore powder of example 8 is prepared by the preparation example C;
the wall-broken ganoderma lucidum spore powder of example 9 was prepared by preparation example D.
Examples 10 to 12
Examples 10 to 12 all relate to a method for preparing a capsule of wall-broken ganoderma lucidum spore powder, all based on example 9, and are different from example 9 only in that ganoderma lucidum fine powder in the step of mixing materials is prepared by different preparation methods, specifically:
the ganoderma lucidum fine powder in the embodiment 10 is prepared by the preparation example b;
the ganoderma lucidum fine powder of example 11 is prepared by the preparation example c;
the ganoderma lucidum fine powder of example 12 is prepared according to preparation example d.
Comparative example
Comparative example 1
A preparation method of a wall-broken ganoderma lucidum spore powder capsule is based on example 6 and is only different from example 6 in that: and in the step P3 of preparing the wall-broken ganoderma lucidum spore powder, drying the spore powder mixture by adopting a vacuum drying process, and controlling the water content of the dried spore powder to be lower than 4%. The vacuum drying temperature is 30 ℃ and the pressure is 0.4 MPa.
Comparative example 2
A preparation method of a wall-broken ganoderma lucidum spore powder capsule is based on example 6 and is only different from example 6 in that: and in the granulating step, drying the total mixed powder by adopting a vacuum drying process after granulating, and controlling the water content of the dried material particles to be lower than 4%. The vacuum drying temperature is 30 ℃ and the pressure is 0.4 MPa.
Comparative example 3
A preparation method of a wall-broken ganoderma lucidum spore powder capsule is based on example 6 and is only different from example 6 in that: and in the step P3 of preparing the wall-broken ganoderma lucidum spore powder, a microwave dryer is adopted to dry the spore powder mixture, and the water content of the dried spore powder is controlled to be lower than 4%. The drying temperature is 50 ℃ and the drying time is 2 h.
Comparative example 4
A preparation method of a wall-broken ganoderma lucidum spore powder capsule is based on example 6 and is only different from example 6 in that: and in the granulating step, drying the total mixed powder by using a microwave dryer after granulating, and controlling the water content of the dried material particles to be lower than 4%. The drying temperature is 50 ℃ and the drying time is 2 h.
Performance test
Detection method
Taking the dried granules as test samples respectively, and carrying out the following detection or test respectively:
(1) determination of polysaccharide content
Preparing a test solution: weighing 1g of the content of the wall ganoderma spore powder capsule (namely the dry material granule obtained in the granulating step), precisely weighing, placing in a round bottom flask, adding 100ml of 80% absolute ethyl alcohol, extracting under reflux at 85 ℃ for 2 times, each time for 0.5h, filtering, discarding the filtrate, adding 100ml of distilled water, extracting under reflux at 100 ℃ for 2 times, each time for 1h, and filtering. Mixing the filtrates, diluting to a volume of 250ml in a volumetric flask, and shaking up to obtain the final product.
Preparation of control solutions: accurately weighing D-anhydrous glucose reference substance 10 dried to constant weight, placing in 100ml measuring flask, and adding distilled water to obtain solution of 0.10 g.L-1The reference solution is put in a refrigerator for standby.
Drawing a standard curve: precisely absorbing 0.3 mL, 0.6 mL, 0.9 mL, 1.2 mL, 1.5 mL and 1.8mL of glucose reference substance solution, respectively placing in a test tube with a plug, adding distilled water to 2.0mL, shaking up, adding 5% phenol solution 1mL and 5% sulfuric acid 5mL in an ice bath, shaking up, standing for 5min, heating in a boiling water bath for 15min, cooling to room temperature, using 2.0mL of distilled water as a blank, carrying out the same method, and measuring the absorbance at the wavelength of 490 nm. And (4) drawing a standard curve by taking the mass concentration (C) as an abscissa and taking A as an ordinate.
And (3) sample content determination: precisely absorbing 2ml of test solution, measuring the absorbance, and substituting into a standard curve to calculate the polysaccharide content. The measurement of each sample of the examples and the comparative examples was averaged 3 times, and the final polysaccharide content was converted to the mass percentage content (%) and recorded.
The test results are reported in table 5.
(2) Measurement of spore oil content
The content of the wall-broken ganoderma lucidum spore powder capsule (namely the dry material particles obtained in the granulation step) of each example and the comparative example was subjected to spore oil extraction and calculated by using an HA121-50-01 supercritical carbon dioxide extraction device (from south China, Jiangsu, China's supercritical extraction Co., Ltd.).
The extraction process flow of the spore oil comprises the following steps: placing the contents of the wall-broken ganoderma lucidum spore powder capsule in a 1L extraction kettle, setting instrument parameters, circularly extracting for a certain time, collecting the oil in a separation kettle I, II, removing impurities, and mixing and weighing.
The content of spore oil (Ganoderma spore oil/wall-broken Ganoderma spore powder capsule) is 100%
Extraction conditions are as follows: the flow rate of carbon dioxide is 20L/h; the extraction pressure is 30MPa, the extraction temperature is 40 ℃, and the extraction time is 2 hours; the pressure of a separation kettle I is 8MPa, and the temperature is 56 ℃; the pressure of the separation kettle II is 4MPa, and the temperature is 36 ℃.
The test results are reported in table 5.
(3) Ergosterol content determination
Referring to GB/T25221-2010 examples and comparative examples, the content of ergosterol in the contents (i.e. dried granules obtained in the granulation step) of the capsule of wall-broken ganoderma lucidum spore powder is disclosed.
The test results are reported in table 5.
TABLE 5 content of effective components in capsule of wall-broken Ganoderma spore powder
From the data in table 5, it can be seen that: the wall-broken ganoderma lucidum spore powder capsule is prepared according to the method, the polysaccharide content of the prepared wall-broken ganoderma lucidum spore powder capsule is as high as 5.53-6.82%, the spore oil content is as high as 25.2-30.8%, and the ergosterol content is as high as 1.2-3.6 mg/kg, so that the wall-broken ganoderma lucidum spore powder prepared by the specific process and the wall-broken ganoderma lucidum spore powder capsule prepared by the specific process can effectively keep functional active ingredients in ganoderma lucidum, and particularly, the ergosterol content is improved most remarkably. Comparing example 6 with comparative examples 1-4, it can be seen that the polysaccharide content, spore oil content and ergosterol content of the capsule prepared by conventional vacuum drying and microwave drying are far lower than those of the capsule prepared by the method of the present application.
(4) Simulated human digestion test
Preparing artificial gastric juice: adding 8.2mL of dilute hydrochloric acid into 400mL of distilled water, adding 5g of pepsin, shaking uniformly, and adding water to dilute to 500 mL;
preparing artificial intestinal juice: adding 250mL of distilled water into 3.4g of monopotassium phosphate, then adding 0.1mol/L of sodium hydroxide solution, and adjusting the pH value to 6.8; dissolving 5g of pancreatin in a proper amount of water; the two solutions were mixed and diluted to 500mL with water.
Pepsin, pancreatin, both from Sigma company, usa; dilute hydrochloric acid was obtained by diluting 3.4mL of hydrochloric acid (36%) to 100 mL.
The contents of the capsule of the wall-broken ganoderma lucidum spore powder (namely the dry granules obtained in the granulation step) of the examples and the comparative examples are respectively treated as follows:
putting 50g of the contents of the capsule of the wall-broken ganoderma lucidum spore powder into a 1000mL conical flask, adding 150mL of artificial gastric juice, and stirring for 5h at the constant temperature of 37 ℃ in a shaking table. Transferring into a centrifugal tube, and centrifuging for 5min at the speed of 4000 r/min. After the supernatant was discarded, 650mL of artificial intestinal juice was added, and the mixture was stirred for 5 hours at a constant temperature of 37 ℃ on a shaker. Transferring into a centrifugal tube, centrifuging at 4000r/min for 5min, and discarding the supernatant. Adding 500ml of distilled water, shaking uniformly, centrifuging at the rotating speed of 4000r/min for 5min, removing supernatant, and drying sediment at the bottom of a centrifuge tube.
After the treatment is finished, the polysaccharide content and the ergosterol content of the contents of the processed wall-broken ganoderma lucidum spore powder capsule are determined by referring to the method, and the absorption rate is calculated according to the following formula.
The absorption rate (1-content after human digestion test/content before human digestion test) × 100%
The measurement results are reported in Table 6.
TABLE 6 table of results of digestion test of simulated human body
From the data in table 6, it can be seen that: the absorption rate of the polysaccharide of the wall-broken ganoderma lucidum spore powder capsule is up to 90.4-96.9%, and the absorption rate of ergosterol is up to 91.6-98.1%, so that the wall-broken ganoderma lucidum spore powder capsule prepared according to the specific process effectively retains the functional active ingredients in ganoderma lucidum, and also has the effect that the functional active ingredients are easily absorbed and utilized by human bodies. Comparing example 6 with comparative examples 1-4, it can be found that the absorption rate of the effective components of the capsule of the wall-broken ganoderma lucidum spore powder prepared by the method is far lower than that of the capsule of the wall-broken ganoderma lucidum spore powder prepared by the method of the application by adopting the conventional vacuum drying and microwave drying in the preparation process.
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Claims (10)
1. A method for preparing a capsule of wall-broken ganoderma lucidum spore powder is characterized by comprising the following steps,
a material mixing step: mixing wall-broken Ganoderma spore powder 94-98% and Ganoderma fine powder 2-6% to obtain total mixed powder;
the wall-broken ganoderma lucidum spore powder is prepared by the following processes:
p1, cleaning the ganoderma lucidum spore powder with clear water to obtain cleaned spore powder; p2, soaking the cleaned spore powder in water, fully stirring again, and filtering to obtain filtrate containing Ganoderma spore powder; standing to allow the filtrate to naturally precipitate until layering, removing supernatant, and retaining the bottom layer spore powder mixture; p3, freeze-drying the spore powder mixture obtained in the step P2 to obtain freeze-dried spore powder, and controlling the water content of the freeze-dried spore powder to be less than 4%; p4, performing wall breaking treatment on the freeze-dried spore powder obtained in the step P3 by using a wall breaking machine to obtain wall-broken ganoderma lucidum spore powder for later use;
wherein the ganoderma lucidum fine powder is prepared by the following process:
s1, soaking the lucid ganoderma fruit bodies or the lucid ganoderma slices in water, washing with water, and draining to obtain the clean lucid ganoderma fruit bodies or the lucid ganoderma slices; s2, adding the cleaned Ganoderma encarpium or Ganoderma slice into water, heating, extracting at 100 deg.C for 0.8-1.2 hr, filtering and retaining the filtrate; extracting under the same conditions for 2 times, mixing filtrates, and concentrating to obtain concentrated filtrate; s3, mixing the concentrated filtrate according to the mass ratio of 1: (2.0-3.0) adding ethanol with the concentration more than or equal to 80% for alcohol precipitation, standing and layering; s4, removing the supernatant liquid of the alcohol precipitation in the step S3, reserving the precipitate, and drying to obtain the ganoderma lucidum fine powder for later use;
a granulation step: granulating the total mixed powder, and freeze-drying to obtain freeze-dried granules, wherein the water content of the freeze-dried granules is controlled to be less than 7%;
and (3) filling capsules: and (4) filling the freeze-dried granules obtained in the granulation step into capsules to obtain the wall-broken ganoderma lucidum spore powder capsules.
2. The method for preparing the wall-broken ganoderma lucidum spore powder capsule according to claim 1, wherein the freeze drying process in the step P3 is as follows:
firstly, under the condition of 0.8MPa of vacuum degree, cooling to-42 to-38 ℃ at the speed of 0.4-0.6 ℃/min, and preserving heat for 1.8-2.2 hours; then, under the condition of the vacuum degree of 1.0MPa, the temperature is raised to 38 to-42 ℃ at the speed of 0.1 to 0.15 ℃/min, and the temperature is kept for 9 to 11 hours.
3. The method for preparing the capsule of wall-broken ganoderma lucidum spore powder according to claim 2, wherein the freeze drying process in the granulating step is as follows:
firstly, under the condition of 0.8MPa of vacuum degree, cooling to-42 to-38 ℃ at the speed of 0.4-0.6 ℃/min, and preserving heat for 1.8-2.2 hours; then, under the condition of the vacuum degree of 1.0MPa, the temperature is raised to 38 to-42 ℃ at the speed of 0.1 to 0.15 ℃/min, and the temperature is kept for 9 to 11 hours.
4. The method for preparing the wall-broken ganoderma lucidum spore powder capsule according to any one of claims 1 to 3, wherein the specific operation steps of the P1 step are as follows:
adding clear water into the ganoderma lucidum spore powder according to the proportion that 70-80 parts by weight of clear water is added into every 3 parts by weight of ganoderma lucidum spore powder, stirring to fully disperse the ganoderma lucidum spore powder, and naturally precipitating for 1.0-2.0 hours; after precipitation, removing the upper clear water and reserving the bottom precipitation mixture; repeating the operation for 4-6 times until no suspended matters exist in the upper clear water, and obtaining the cleaned spore powder.
5. The method for preparing the capsule of sporoderm-broken ganoderma lucidum spore powder according to claim 4, wherein in the step of P2:
adding the cleaned spore powder into 70-80 parts of clear water, soaking for 1.0-2.0 hours, fully stirring again, and filtering.
6. The method for preparing the capsule of sporoderm-broken ganoderma lucidum spore powder according to claim 4, wherein in the step of P2:
adopts double-layer filter screens for filtration, the mesh number of the first layer filter screen is 90-110 meshes, and the mesh number of the second layer filter screen is 190-210 meshes.
7. The method for preparing wall-broken ganoderma lucidum spore powder capsules according to any one of claims 1 to 3, wherein in the step of P4:
and (3) the temperature of circulating cooling water of the wall breaking machine is less than 22 ℃, the feeding amount is 1.8-2.2 kg each time, and the obtained wall-broken ganoderma lucidum spore powder is vacuum-packaged for later use.
8. The method for preparing wall-broken ganoderma lucidum spore powder capsules according to any one of claims 1 to 3, wherein in the step S1:
soaking Ganoderma fruiting body or Ganoderma slice in water for 20-30min, wherein the water is added in an amount of 20-25 weight parts per 1 weight part of Ganoderma fruiting body or Ganoderma slice.
9. The method for preparing wall-broken ganoderma lucidum spore powder capsules according to claim 8, wherein in the step of S2:
adding cleaned Ganoderma encarpium or Ganoderma slice into 13-17 weight parts of water, heating and extracting, filtering, and retaining filtrate; repeatedly extracting for 2-5 times under the same conditions, combining the filtrates, and concentrating to obtain the final product with Baume degree of 1.0-1.4.
10. A capsule of wall-broken ganoderma lucidum spore powder is characterized in that: the preparation method of the capsule of sporoderm-broken ganoderma lucidum spore powder of any one of claims 1 to 9.
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| CN114272308A (en) * | 2022-02-19 | 2022-04-05 | 姚远平 | A Chinese medicinal composition for treating cancer, and its preparation method |
| CN115338001A (en) * | 2022-08-12 | 2022-11-15 | 武夷山元生泰生物科技有限公司 | Wall breaking method of ganoderma lucidum spore powder |
| CN115381790A (en) * | 2022-08-08 | 2022-11-25 | 广东润源中天生物科技有限公司 | Preparation method of wall-broken ganoderma lucidum spore powder capsule and wall-broken ganoderma lucidum spore powder capsule |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112772825A (en) * | 2021-01-04 | 2021-05-11 | 山西昇力元生物科技有限公司 | Method for reducing heavy metal cadmium in ganoderma lucidum spore powder |
| CN114272308A (en) * | 2022-02-19 | 2022-04-05 | 姚远平 | A Chinese medicinal composition for treating cancer, and its preparation method |
| CN115381790A (en) * | 2022-08-08 | 2022-11-25 | 广东润源中天生物科技有限公司 | Preparation method of wall-broken ganoderma lucidum spore powder capsule and wall-broken ganoderma lucidum spore powder capsule |
| CN115338001A (en) * | 2022-08-12 | 2022-11-15 | 武夷山元生泰生物科技有限公司 | Wall breaking method of ganoderma lucidum spore powder |
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