CN104644697B - The preparation method and applications of ganoderma lucidum Ultramicro-powder - Google Patents
The preparation method and applications of ganoderma lucidum Ultramicro-powder Download PDFInfo
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Abstract
The present invention provides the preparation method and applications of ganoderma lucidum Ultramicro-powder.The present invention provides 3 kinds of preparation methods, methods 1）, direct ultramicro grinding；Method 2）, ganoderma lucidum elder generation water, which carries, obtains ganoderma lucidum water extract, is uniformly mixed with ganoderma lucidum residue Ultramicro-powder afterwards, is prepared into ganoderma lucidum Ultramicro-powder；Method 3）, ganoderma lucidum elder generation alcohol extracting obtains ganoderma lucidum alcohol extract, uniformly mixed with ganoderma lucidum residue Ultramicro-powder afterwards, be prepared into ganoderma lucidum Ultramicro-powder.The average grain diameter of ganoderma lucidum Ultramicro-powder is between 100~900nm.The present invention provides tablet, capsule, the formula of particle and its preparation process of ganoderma lucidum Ultramicro-powder on the basis of ganoderma lucidum Ultramicro-powder, new preparation process, the active constituent content for solving existing ganoderma lucidum class product formula is low, the problem of complex production process, and ganoderma lucidum utilization rate is increased, increase productivity efficiency.And the product of preparation is detected, it was demonstrated that the high conclusion of the active constituent content of ganoderma lucidum Ultramicro-powder product.
Description
Technical field
The invention belongs to processing technique of Chinese herbs and formulation art, and in particular to a kind of antitumor, hypoglycemic ganoderma lucidum ultra micro
The preparation method and its preparation process of powder.
Background technology
Ganoderma lucidum is also known as polyporus lucidus, refreshing sesame, sesame grass, celestial grass, seocho, is the complete stool of Polyporaceae plant red sesame or purple sesame.
Know that Ganoderma (Ganoderma) fungi about more than 100 is planted, distribution is most wide for red sesame (G.lu-cidum), is secondly purple sesame
(G.japonicum), also artist's conk (G.applana-tum), Ganoderma tsugae (G.tsugae) and book tree sesame (G.capense) etc.
Equal hyoscine.《Compendium of Materia Medica》Described in：Ganoderma lucidum bitter, flat, nontoxic, invigorating heart gas, promoting blood circulation enter heart hyperemia, the heart are helped to fill arteries and veins, pacify
God, beneficial lung qi, tonifying liver gas, bowl spares increase wisdom, good color, sharp joint, hard muscles and bones, eliminating the phlegm, stomach invigorating.It is tens of by scientific research institution
The modern pharmacology research in year confirms that ganoderma lucidum adjusts blood glucose, control blood pressure, putting of adjuvant therapy for enhancing body immunity
It treats, liver protecting, sleep etc. is promoted to be respectively provided with significant curative effect.2010 editions pharmacopeia record ganoderma lucidum nature and flavor：Sweet and neutral.The thoughts of returning home,
Lung, liver and kidney channel.Invigorating qi for tranquilization, it is relieving cough and asthma.For having no peace of mind, palpitaition of having a sleepless night, deficiency syndrome of the lung cough and asthma, consumptive disease is losed heart, apathy to drink
Food.Dosage is 6~12g.
Ultramicro-powder is substantially distinguished from general particle and biography with its " bulk effect " (i.e. quantum optical field) and " skin effect "
The block materials of system become a kind of new state existing for substance.From physics angle come divide people by grain size be less than 0.1 μm
Powder is known as Ultramicro-powder；People are divided from ergonomic point, and less than 0.5 μm of powder is called Ultramicro-powder.Chinese medicine (plant)
For cell dia usually at 10~200 μm or so, it is 48 μm (300 that the grain size of Chinese herbal medicine ultra-fine powder, which can generally be crushed to cell grain size,
Mesh)~the powder of 25 μm (500 mesh) in addition it is water-soluble in drink.Many Chinese medicines can be carried out ultramicro grinding, in becoming
Medicinal material Ultramicro-powder.Contained effective substance will not be sent out compared with traditional Chinese medicine medicine materical crude slice, Chinese medicine preparation in ultra micro Chinese medicine
Variation on raw apparent molecular structure, will not lead to the change of Chinese medicine attribute, pharmacodynamic properties and major function, be herbal medicine efficacy
Basic guarantee is provided with stabilization.
Ultra-fine powder technology is a kind of new crushing technology to grow up to adapt to modern technology requirements, and material is through super
After refinement, there is minimum volume, thus it is easily attached to the surface of other substances and expands to the inside of these substances rapidly
Infiltration is dissipated, physically or chemically effect formation, which occurs, with the surface of other substances closely combines, and obtains very curative effect.Ultramicro-powder has
Be conducive to retain bioactive ingredients, improve dissolution rate, reduce the difference of drug effect formed due to absorption of human body difference, improve
Drug effect saves the features such as material resources, suitable for Chinese medicine [Fang Bangjiang, the Chen Hao of herb resource not extensively, more than residue active ingredient
Wait the advantage of Chinese herbal ultra-fine powders and application prospect China traditional Chinese medicine modern distance education .2010,8 (18):208-209].Ganoderma lucidum
Human body can improve its absorptivity 45 times after conidia powder super-micro wall-broken, but oxygen easily occurs for the lucidum spore powder after super-micro wall-broken
Change and go bad, oxidation rate is 2500 times of the lucidum spore powder without broken wall.So lucidum spore powder is unsuitable for ultramicro grinding.
And ganoderma lucidum resource shortage and residue active ingredient is more, oxidation deterioration is not susceptible to, ultra micro powdering techniques are suitable for ganoderma lucidum.Dong Yining
A kind of " preparation method of lucid ganoderma solid beverage " patent (application No. is 201410157714.3) of applications is waited to propose that ganoderma lucidum is real
Body Ultramicro-powder grain size is 20~50 μm；" a kind of super-micro wall-broken glossy ganoderma composition and preparation method thereof " patent (Shen of Shi Meng applications
Please number for 201410316806.1) propose powder diameter in 0.01 μm~150 μ ms；A kind of " nothing of the applications such as Shen Lirong
The patent (application No. is 201110420345.9) of the Preparation method and use of public hazards ganoderma lucidum Ultramicro-powder " proposes powder average particle size
100% reaches 9.96 μm hereinafter, median D50 is 2.92 μm；It can be seen that the particle size range of prior art is at 0.01 μm~150 μm
Interior, particle size range span is big, particle is uneven, and the utilization rate of active ingredient is low, and process costs are high.
Invention content
The purpose of the present invention is to overcome the deficiencies of the prior art, provide a kind of ganoderma lucidum Ultramicro-powder preparation method and its
Using.
The present invention includes following technical solution：
Technical solution 1：Provide a kind of preparation method of ganoderma lucidum Ultramicro-powder, obtain ganoderma lucidum average grain diameter for 100~
900nm includes the following steps：
1) using ganoderma lucidum as raw material, impurities removing is cleaned 3~5 times, hydraulic pressure 10MPa with drinking water, by cleaned ganoderma lucidum into
Row slice, then below coarse powder to 80 mesh；
2) the good ganoderma lucidum powder of coarse powder is subjected to ultra-fine grinding using the impact grinding of high energy nanometer, passes through high energy nanometer impact grinding
Mill in tank body is situated between ceaselessly impacting 6~10 hours, and the average grain diameter of ganoderma lucidum Ultramicro-powder is made to reach 100~900nm.
Technical solution 2：Provide a kind of preparation method of ganoderma lucidum Ultramicro-powder, obtain ganoderma lucidum average grain diameter for 100~
900nm includes the following steps：
1) feedstock processing：Using ganoderma lucidum as raw material, it will wherein sundries reject, be cleaned 3~5 times, hydraulic pressure 10MPa with drinking water,
Ganoderma lucidum is sliced；
2) water carries：The ganoderma lucidum of step 1) is placed in extractor after boiling and keeps boil condition 1 hour, filtering is filtered clever
Sesame Aqueous extracts and ganoderma lucidum residue.Ganoderma lucidum residue is added in into distilled water, boil condition 30min is kept after boiling, ganoderma lucidum is filtered to obtain in filtering
Aqueous extracts and ganoderma lucidum residue A；
3) Aqueous extracts are dried：The ganoderma lucidum Aqueous extracts of step 2) are merged, is placed in Rotary Evaporators, 60 DEG C~80 DEG C, subtracts
Pressure rotary evaporation is concentrated to dryness medicinal extract, after letting cool, is put into vacuum drying chamber, 40~55 DEG C of vacuum drying obtain ganoderma lucidum water for 24 hours
Extract；
4) drying of ganoderma lucidum residue and coarse powder：The ganoderma lucidum residue A of step 2) is placed at room temperature for drying, then be placed in vacuum drying
In case, 60 DEG C are dried in vacuo 24 hours, take out, put it into and coarse powder is carried out in pulverizer；
5) ganoderma lucidum Ultramicro-powder：The ganoderma lucidum water extract of step 3) and the coarse powder of step 4) are merged, is put into blender and mixes
It is even, then ultramicro grinding is carried out to consolidated material with micronizer, it is ceaselessly hit by mill Jie in high energy nanometer impact grinding tank body
It hits grinding 6~10 hours, the average grain diameter of ganoderma lucidum Ultramicro-powder is made to reach 100~900nm.
Technical solution 3：Provide a kind of preparation method of ganoderma lucidum Ultramicro-powder, obtain ganoderma lucidum average grain diameter for 100~
900nm includes the following steps：
1) feedstock processing：Using ganoderma lucidum as raw material, it will wherein sundries reject, be cleaned 3~5 times, hydraulic pressure 10MPa with drinking water,
Ganoderma lucidum is sliced；
2) alcohol extracting：The ganoderma lucidum of step 1) is added into 75% ethyl alcohol, is heated to reflux 45min, filters, filters to obtain ganoderma lucidum alcohol extract and spirit
Sesame residue.Ganoderma lucidum residue is added in into 75% ethyl alcohol, is heated to reflux 45min, filters, filters to obtain ganoderma lucidum alcohol extract and ganoderma lucidum residue A；
3) ganoderma lucidum alcohol extract is dried：The ganoderma lucidum alcohol extract of step 2) is merged, is placed in Rotary Evaporators, 60 DEG C~80
DEG C, rotary evaporation is depressurized, obtains ganoderma lucidum alcohol extracting thing；
4) drying of ganoderma lucidum residue and coarse powder：The ganoderma lucidum residue A of step 2) is placed at room temperature for drying, then be placed in vacuum drying
In case, 40~55 DEG C are dried in vacuo 24 hours, take out, put it into and coarse powder is carried out in pulverizer；
5) ganoderma lucidum Ultramicro-powder：The coarse powder of the ganoderma lucidum alcohol extracting thing of step 3) and step 4) is merged, is put into blender and mixes
It is even, then ultramicro grinding is carried out to consolidated material with micronizer, it is ceaselessly hit by mill Jie in high energy nanometer impact grinding tank body
It hits grinding 6~10 hours, the average grain diameter of ganoderma lucidum Ultramicro-powder is made to reach 100~900nm.
Technical solution 4：A kind of preparation method for the tablet that ganoderma lucidum Ultramicro-powder is prepared containing the above method is provided, including such as
Lower step：Ganoderma lucidum Ultramicro-powder, starch, sodium carboxymethylcellulose and stearic acid are uniformly mixed, is dissolved and made with appropriate 95% ethyl alcohol
Grain is put into vacuum drying chamber and is dried under vacuum to water content 3% hereinafter, then crushing the piece of drying and/or block for 60 DEG C
Then particle into below 14 mesh adds in magnesium stearate mixing, cross 12 mesh sieve whole grain, be pressed into plain piece, then wrap up waterproofing membrane
Clothing.
Technical solution 5：A kind of preparation method for the capsule that ganoderma lucidum Ultramicro-powder is prepared containing the above method is provided, including such as
Lower step：30min is mixed in ganoderma lucidum Ultramicro-powder and magnesium stearate, is dissolved and pelletized with appropriate 95% ethyl alcohol, be put into vacuum and do
In dry case water content 3% is dried under vacuum to hereinafter, then the piece of drying and/or block to be ground into below 14 mesh for 60 DEG C
Grain sieves whole grain after 12 mesh, is packed into gelatin hollow capsule, packs.
Technical solution 6：A kind of preparation method for the particle that ganoderma lucidum Ultramicro-powder is prepared containing the above method is provided, including such as
Lower step：Ganoderma lucidum Ultramicro-powder, starch, sodium carboxymethylcellulose and stearic acid are uniformly mixed, is dissolved and made with appropriate 95% ethyl alcohol
Grain is put into vacuum drying chamber and is dried under vacuum to water content 3% hereinafter, then crushing the piece of drying and/or block for 60 DEG C
Then particle into below 14 mesh adds in magnesium stearate mixing, cross 12 mesh sieve whole grain, granule packaging.
Technical solution 7：Provide the ganoderma lucidum Ultramicro-powder of above method preparation, in the ganoderma lucidum Ultramicro-powder, ganoderma lucidum polysaccharide
Content not less than 0.57%, the content of ganodenic acid is not less than 1.19%.
Technical solution 8：The ganoderma lucidum Ultramicro-powder of above method preparation is provided in antitumor, hypoglycemic drug is prepared
Using.
The present invention has the following technical effect that：
Technical scheme of the present invention 1 provides the production technology that a kind of ganoderma lucidum Ultramicro-powder average grain diameter is 100~900nm,
And technique has met the standard of Ultramicro-powder, grain size is invented less than other, and particle is relatively uniform, improve active ingredient dissolution rate and
Its drug effect, reduces production cost.
Technical scheme of the present invention 2 and 3 is fully extracted for effective component of glossy ganoderma and has carried out technological innovation.Ganoderma lucidum mainly into
It is divided into ganoderma lucidum polysaccharide and ganodenic acid, main extracting method is carried for water or ethyl alcohol extraction [Liu Jia, Wang Yong the spirits of different solubility
The progress modern medicines of sesame polysaccharide and clinic .2012,27 (6)], [Jiang Tingting, Wang Yong.The research of Ganoderma lucidum triterpenes components
Be in progress Strait Pharmaceutical Journals .2014,24 (1)].But these methods all do not extract ganoderma lucidum fully, the active ingredient of ganoderma lucidum is not
But it is present in extracting solution, also has in residue and [open Man, orchid ganoderma lucidum polysaccharide is isolated and purified with pharmacological activity and in function
Food research and developments, 2005,2 (26) are applied in food:118-120], and its main component of ganoderma lucidum also have alkaloid,
[the purple sesames such as horse high official position, Luo Ying, the magnificent swallow chemistry such as long alkenoic acid, lactones, coumarin, water soluble protein, ergosterol, resin
The progress International Journal of Triditional Chinese Medicines .2012.34 (11) of ingredient and pharmacological activity], technical solution of the present invention 2 and 3 passes through
Experiment ganoderma lucidum water is carried or alcohol extracting after the residue left be detected, it is found that it contains these substances, resource kept to maximize
Residue after extraction has also been carried out ultramicronising crushing, while glossy ganoderma ultra-fine powder by the attitude utilized, technical solution of the present invention 2 and 3
It is the product merged by water carries or alcohol extracting obtains extract and later stage residue Ultramicro-powder early period, this technique not only saves material
Expect resource, and improve ganoderma lucidum drug effect.
Technical scheme of the present invention 4,5,6 provides a kind of carry water or extraction powder and later stage residue that alcohol extracting obtains surpass
The novel material of the mixed uniformly ganoderma lucidum Ultramicro-powder of micro mist.Commercially available ganoderma lucidum product dosage form is mostly tablet, capsule, particle, oral liquid,
With lucidum spore powder, ganoderma lucidum mycelium powder, (a kind of ganoderma lucidum chewable tablet of Zhao Yuncai, Li Na, Zhao Shanshan, Tan Yi apply mostly
Number：201310570469.4), ganoderma lucidum Ultramicro-powder [applications such as Zhang Sufeng " dendrobium candidum, Cordyceps militaris, ganoderma lucidum and tealeaves compound
Ganoderma lucidum Ultramicro-powder is the full powder of ganoderma lucidum plant and grain in the patent (application No. is 201410159981.4) of chewable tablets and preparation method "
Diameter is less than 300 mesh] as raw material, and most products auxiliary material accounting is high, type is various such as " coffee with ganoderma lucidum " of Hu Haiyan applications
Patent (application number 201410310150.2) formula for 0.2% salt, 0.2% calcium phosphate, 0.2% carragheen, 0.4% coffee
Powdered flavor, 9% instant coffee powder, 10% whole-fat milk powder, 20% vegetable fat powder, 35% ganoderma particles, 25% white granulated sugar, Feng Peng etc.
Lucidum spore powder accounts in the patent (application No. is 200610040558.8) of " ganoderma spore tablet and its preparation process " of application
20%.Material content is high in inventive formulation, and all very stable through lab scale, pilot scale, big trial work skill.
Technical solution 7：By detecting ganoderma lucidum polysaccharide in ganoderma lucidum Ultramicro-powder using Chinese Pharmacopoeia ganoderma lucidum polysaccharide detection method
The content that content measures ganodenic acid in ganoderma lucidum Ultramicro-powder not less than 0.57% and using spectrophotometry is not less than 1.19%.Recklessly
Patent (the application number of " a kind of high efficiency preparation method of ganoderma lucidum polysaccharide " of the applications such as Qiu Hui：200810156039.7) in propose its
Yield is 20.79% or so, hot water leaching 16.2 or so, a kind of ganoderma lucidum polysaccharide and the preparation method and application (patent No.：
ZL03116403.X) gained yield is 9.7%；Application number：201110261149.1 (such as Jinsong ZHANG, Zhang Hui, Tang Chuanhong are a kind of
The method of extracting triterpenoids from ganoderma lucidum sporocarp) in show that its peculiar method extraction yield is up to 0.66%, ethyl alcohol extraction
It is 0.66% to take highest yield.The yield of the present invention is higher than the yield of common flour.
Technical solution 8：The ganoderma lucidum Ultramicro-powder of above method preparation is provided in antitumor, hypoglycemic drug is prepared
Using and apply when it is safe and non-toxic.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail.
Embodiment 1 prepares ganoderma lucidum Ultramicro-powder
The method that ganoderma lucidum Ultramicro-powder is prepared in the present embodiment, is as follows：
1) using ganoderma lucidum as raw material, impurities removing is cleaned 3~5 times, hydraulic pressure 10MPa with drinking water, by cleaned ganoderma lucidum into
Row slice, then below coarse powder to 80 mesh.
2) the good ganoderma lucidum powder of coarse powder is subjected to ultra-fine grinding using the impact grinding of high energy nanometer, passes through high energy nanometer impact grinding
Mill in tank body is situated between ceaselessly impacting 6~10 hours, and the average grain diameter of ganoderma lucidum Ultramicro-powder is made to reach 100~900nm.
Production detailed data is shown in Table 1：
Table 1
| Product batch number | Raw material dosage (kg) | Output (kg) | Waste (%) | Yield (%) | Average grain diameter (nm) |
| 140918-1 | 5.01 | 4.86 | 3.04 | 96.96 | 100~900nm |
| 140918-2 | 4.99 | 4.84 | 2.98 | 97.02 | 100~900nm |
| 140918-3 | 4.98 | 4.83 | 3.02 | 96.98 | 100~900nm |
(remarks：This 3 lot number techniques are identical, and raw material dosage is different.)
Embodiment 2 prepares ganoderma lucidum Ultramicro-powder
The method that ganoderma lucidum Ultramicro-powder is prepared in the present embodiment, is as follows：
1) feedstock processing：Using ganoderma lucidum as raw material, it will wherein sundries reject, be cleaned 3~5 times, hydraulic pressure 10MPa with drinking water,
Ganoderma lucidum is sliced, is put into extractor；
2) water carries：Add distilled water 5, the ganoderma lucidum of step 1 is placed in extractor after boiling and keeps boil condition 1 hour, mistake
Filter, filters to obtain ganoderma lucidum Aqueous extracts and ganoderma lucidum residue.Ganoderma lucidum residue is added in into distilled water, boil condition 30min, mistake are kept after boiling
Filter, filters to obtain ganoderma lucidum Aqueous extracts and ganoderma lucidum residue A；
3) Aqueous extracts are dried：The ganoderma lucidum Aqueous extracts of step 2) are merged, is placed in Rotary Evaporators, 60 DEG C~80 DEG C, subtracts
Pressure rotary evaporation is concentrated to dryness medicinal extract, after letting cool, is put into vacuum drying chamber, 40~55 DEG C of vacuum drying obtain ganoderma lucidum water for 24 hours
Extract；
4) drying of ganoderma lucidum residue and coarse powder：The ganoderma lucidum residue A of step 2) is placed at room temperature for drying, then be placed in vacuum drying
In case, 60 DEG C are dried in vacuo 24 hours, take out, put it into and coarse powder is carried out in pulverizer；
5) ganoderma lucidum Ultramicro-powder：The ganoderma lucidum water extract of step 3) and the coarse powder of step 4) are merged, are put into mixing in blender,
Ultramicro grinding is carried out to consolidated material with micronizer again, is situated between ceaselessly to hit by the mill in high energy nanometer impact grinding tank body and grind
Mill 6~10 hours, makes the average grain diameter of ganoderma lucidum Ultramicro-powder reach 100~900nm.
Production detailed data is shown in Table 2：
Table 2
| Product batch number | Raw material dosage (kg) | Output (kg) | Waste (%) | Yield (%) | Grain size (nm) |
| 140919-1 | 0.98 | 0.92 | 6.01 | 93.99 | 100~900nm |
| 140919-2 | 1.05 | 0.99 | 6.04 | 93.96 | 100~900nm |
| 140919-3 | 1.03 | 0.97 | 5.98 | 94.02 | 100~900nm |
(remarks：This 3 lot number techniques are identical, and raw material dosage is different.)
Embodiment 3
The method that ganoderma lucidum Ultramicro-powder is prepared in the present embodiment, is as follows：
1) feedstock processing：It is high-quality with quality, it is raw material without the ganoderma lucidum to go mouldy, will wherein sundries rejects, 3 are cleaned with drinking water
~5 times, ganoderma lucidum is sliced, is put into extractor by hydraulic pressure 10MPa；
2) alcohol extracting：The ganoderma lucidum of step 1) is added into 75% ethyl alcohol 50L, is heated to reflux 45min, filters, filters to obtain ganoderma lucidum alcohol extract
With ganoderma lucidum residue.Ganoderma lucidum residue is added in into 75% ethyl alcohol 25L, is heated to reflux 45min, filters, filters to obtain ganoderma lucidum alcohol extract and ganoderma lucidum
Residue A；
3) ganoderma lucidum alcohol extract is dried：The ganoderma lucidum alcohol extract of step 2) is merged, is placed in Rotary Evaporators, 60 DEG C~80
DEG C, rotary evaporation is depressurized, obtains ganoderma lucidum alcohol extracting thing；
4) drying of ganoderma lucidum residue and coarse powder：The ganoderma lucidum residue A of step 2) is placed at room temperature for drying, then be placed in vacuum drying
In case, 40~55 DEG C are dried in vacuo 24 hours, take out, put it into and coarse powder is carried out in pulverizer；
5) ganoderma lucidum Ultramicro-powder：The coarse powder of the ganoderma lucidum alcohol extracting thing of step 3) and step 4) is merged, is put into blender and mixes
It is even, then ultramicro grinding is carried out to consolidated material with micronizer, it is ceaselessly hit by mill Jie in high energy nanometer impact grinding tank body
It hits grinding 6~10 hours, the average grain diameter of ganoderma lucidum Ultramicro-powder is made to reach 100~900nm.
Production detailed data is shown in Table 3：
Table 3
(remarks：This 3 lot number techniques are identical, and raw material dosage is different.)
Embodiment 4
Ganoderma lucidum Ultramicro-powder 25g, 18g starch of Example 1,2,3,1.5g sodium carboxymethylcelluloses, 1.5g are stearic respectively
Acid is uniformly mixed, and is dissolved and pelletized with appropriate 95% ethyl alcohol, be put into vacuum drying chamber 60 DEG C be dried under vacuum to water content 3% with
Under, the piece of drying and/or block are then ground into particle below 14 mesh, then add in 0.4g magnesium stearate mixings, mistake
12 mesh sieve whole grain, are pressed into the plain piece 100 of 0.5g, quality inspection, then wrap up waterproofing membrane clothing up to ganoderma lucidum submicron powder sheet.
Embodiment 5
30min is mixed in ganoderma lucidum Ultramicro-powder 2.97g, the 300mg magnesium stearate of Example 1,2,3 respectively, with appropriate
The dissolving granulation of 95% ethyl alcohol, is put into vacuum drying chamber and is dried under vacuum to water content 3% hereinafter, then by the piece of drying for 60 DEG C
And/or block is ground into the particle below 14 mesh, sieves whole grain after 12 mesh, is packed into gelatin hollow capsule, packs to obtain 300mg
Ganoderma lucidum Ultramicro-powder capsule finished product 100, quality inspection.
Embodiment 6
Ganoderma lucidum Ultramicro-powder 25g, 18g starch of Example 1,2,3,1.5g sodium carboxymethylcelluloses, 0.5g are stearic respectively
Acid is uniformly mixed, and is dissolved and pelletized with appropriate 95% ethyl alcohol, be put into vacuum drying chamber 60 DEG C be dried under vacuum to water content 3% with
Under, the piece of drying and/or block are then ground into particle below 14 mesh, then add in 0.4g magnesium stearate mixings, mistake
12 mesh sieve whole grain, and 100 bags of granule packaging, quality inspection is to get ganoderma lucidum ultrafine powder particle.
Embodiment 7
Ganoderma lucidum Ultramicro-powder and common flour ganoderma lucidum polysaccharide and ganodenic acid determination study
1 instrument and material
1.1 instrument
Electric-heated thermostatic water bath (Zhengzhou Great Wall), ultraviolet specrophotometer (Shimadzu UV-2600), electronic balance (Sai Duoli
This CPA225D), Soxhlet extractor, electric heater (Zhengzhou Great Wall DRT-SX), ultrasonic cleaner (Kunshan Shu Mei KQ-300)
1.2 drugs and reagent
Glucose control product (Nat'l Pharmaceutical ＆ Biological Products Control Institute, lot number 20051126), ursolic acid standard items (China
Pharmaceutical biological product examine and determine institute, lot number 110709-200304), ganoderma lucidum Ultramicro-powder (raw material sources for claims 1 to 3 it is arbitrary
The method of one prepares ganoderma lucidum Ultramicro-powder) and Common ganoderma lucidum powder (ganoderma lucidum is selected, cleaning, slice, it is dry, crush, cross 100 mesh
Sieve gained), anthrone, sulfuric acid, vanillic aldehyde, glacial acetic acid, perchloric acid, ethyl acetate be analysis it is pure
2 ganoderma polyoses contents measure
The preparation of 2.1 solution
2.1.1 the preparation of reference substance solution takes glucose control product appropriate, accurately weighed, adds water that every 1ml is made containing 0.1mg
Solution to get.
2.1.2 the preparation precision of sulfuric acid anthrone solution weighs anthrone 0.1g, adds 80% sulfuric acid solution 100ml to make dissolving,
Shake up to get.
The preparations of 2.2 standard curves respectively it is accurate measure reference substance solution 0.2ml, 0.4m1,0.6ml, 0.8ml, 1.0ml,
1.2ml is put in 10ml tool plug test tubes, adds water to 2.0ml, and precision adds in sulfuric acid anthrone solution 6ml, shakes up, put in water-bath and heat
15min takes out, is put into ice bath and cools down 15min, and using corresponding reagent as blank, absorbance is measured at 625nm wavelength, with
Absorbance is ordinate, a concentration of abscissa, draws standard curve.
The preparation of 2.3 test solutions takes ganoderma lucidum common flour or Ultramicro-powder about 2g, accurately weighed, puts in Soxhlet extractor,
Adding water 90ml, electric heater heating and refluxing extraction to extracting liquid colourless, extracting solution is transferred in 100ml measuring bottles, adds water to scale,
It shakes up.Precision measures 10ml, adds in ethyl alcohol 150ml, shakes up, and 4 DEG C are placed 12 hours, are taken out, and centrifugation, incline supernatant, precipitation
Be dissolved in water, be transferred in 50ml measuring bottles, add water to scale, shake up to get.
2.4 measuring method precisions measure test solution 2ml, put in 10ml tool plug test tubes, and precision adds in sulfuric acid anthrone solution
6ml shakes up, and puts in water-bath and heats 15 minutes, takes out, puts in people's ice bath and cool down 15 minutes, using corresponding reagent as blank,
Absorbance is measured at 625nm wavelength, the weight (mg) containing glucose in test solution is read from standard curve, is calculated, i.e.,
.This product is calculated by dry product, containing ganoderma lucidum polysaccharide with DEXTROSE ANHYDROUS (C6H12O6) meter.
The measure of 3 ganodenic acids
3.1 ursolic acid reference substance solution precisions weigh and the ursolic acid reference substance one of 12 hours are dried under reduced pressure through phosphorus pentoxide
It is quantitative, it puts in volumetric flask, is dissolved with ethyl acetate, ultrasonic 15min, and scale is diluted to, it shakes up, the control of 0.1mg/ml is made
Product solution.
The draftings of 3.2 standard curves respectively it is accurate draw 0.05ml, 0.10ml, 0.30ml, 0.50ml, 0.70ml,
0.90ml reference substance solutions are in 10ml test tubes, after being evaporated in 100 DEG C of water-baths, add in 5% vanillic aldehydes of 0.20ml-glacial acetic acid
It with 1.0ml perchloric acid, shakes, 20min is heated in 60 DEG C of water-baths and moves into 3min is cooled down in ice-water bath, adds 5.00ml ice
Acetic acid shakes up and is placed in room temperature.The absorbance for measuring reference substance solution under 548nm wavelength with spectrophotometer is used after 15min.
It is respectively that ordinate draws standard curve by abscissa and absorbance value of ursolic acid quality.
The preparations of 3.3 sample solutions and measure take ganoderma lucidum Ultramicro-powder sample 0.1g, accurately weighed, put in 100ml volumetric flasks,
It is dissolved with ethyl acetate, ultrasonic 30min, and is diluted to scale, shaken up, filtered.Precision draws 1.0ml filtrates in the test tube of 10ml
In, after being evaporated in 100 DEG C of water-baths, 5% vanillic aldehydes of 0.20ml-glacial acetic acid and 1.0ml perchloric acid are added in, is shaken, in 60 DEG C of water
20min is heated in bath and is moved into, 3min is cooled down in ice-water bath, added 5.00ml glacial acetic acid, shake up and be placed in room temperature.After 15min
With the absorbance of spectrophotometer determination sample solution under 548nm wavelength.
3.4 content calculation ganodenic acids (in terms of ursolic acid)=sample is equivalent to amount (mg)/sample weight (mg) of reference substance
× 100%, as shown in table 4：
Ganoderma lucidum polysaccharide and the content of ganodenic acid in the 4 made glossy ganoderma powder of various techniques of table
(remarks：3 lot number techniques of this common flour are identical, and raw material dosage is different.)
8 ganoderma lucidum Ultramicro-powder antitumor action of embodiment
1 material
1.1 test medicine
Glossy ganoderma powder (source prepares ganoderma lucidum Ultramicro-powder for the method for common flour and Examples 1 to 3 any one), cis-platinum injections
Liquid (Jiangsu Haosen Pharmaceutical Co., Ltd), physiological saline (Harbin No.6 Pharmaceutical Factory).
1.2 experimental animal
Kunming mouse, 18~22g of weight, male and female dual-purpose, university of TCM of Heilongjiang Province animal experimental center provide.
H22 (liver cancer) is purchased from attached tumour hospital of Harbin Medical University.
2 methods
The preparation of 2.1 glossy ganoderma powder Aqueous extracts takes glossy ganoderma powder, and (source is common flour and the method for Examples 1 to 3 any one
Prepare ganoderma lucidum Ultramicro-powder), 15 times of 20~25 DEG C of distilled water immersion 3Omin are added in, filtering retains filtrate；Filter residue adds in 15 times 20
~25 DEG C of distilled water immersion 30min, filtering retain filtrate；Filter residue adds in 10 times of distilled water, with hydrochloric acid tune pH value to 1；Heating is anti-
2h is answered, is let cool, adds in sodium hydroxide tune pH value to 7, filtering obtains filtrate.Merge 3 filtrates, be concentrated into 100% and (be equivalent to 1g
Crude drug/ml), it is tested with normal saline dilution to required concentration.
The foundation of 2.2 mouse tumor models
Take healthy mice, weight 18~22g half male and half females.Intraperitoneal inoculation 7d is selected, well-grown lotus H22 liver cancer
Mouse, cervical dislocation are put to death, aseptic aspiration ascites, and 1 is pressed with sterile saline：2 dilution proportions are into 5.4 × 107/ mL oncocytes
Suspension, it is subcutaneous to be inoculated in healthy mice right fore armpit, every 0.2mL inoculation.
2.3 experiment packet
Next day is inoculated with, is randomly divided into 15 groups, half male and half female, every group of 12 mouse.Respectively negative control group；Physiological saline
Group；Positive controls；Cis-platinum group；Common ganoderma lucidum powder low (50mg/kg), in (100mg/kg), high (200mg/kg) dosage group；It is real
Apply 1 glossy ganoderma powder of example low (50mg/kg), in (100mg/kg), high (200mg/kg) dosage group；Low (the 50mg/ of 2 glossy ganoderma powder of embodiment
Kg (100mg/kg), high (200mg/kg) dosage group in),；3 glossy ganoderma powder of embodiment low (50mg/kg), in (100mg/kg), high
(200mg/kg) dosage group.
2.4 dosages and approach
The daily 100mg/kgBW gastric infusions of each glossy ganoderma powder Aqueous extracts group 1 time, continuous 10d；Positive controls (cis-platinum
Group) for 50mg/ (kgd) is injected intraperitoneally, it is administered once, is administered 3 times altogether, negative control group gavage gives normal salt every other day
Water, one time a day, continuous 10d.
The influence of 2.5 pairs of H22 type mice with tumor tumor suppressions
Tumor tissue is stripped in the mouse of cervical dislocation execution for 24 hours after the last administration to weigh, calculating tumour inhibiting rate, tumour inhibiting rate (%)=
(the T/C of (1-T/C) × 100%：Treatment group's average knurl weight/blank control group average knurl weight).It the results are shown in Table 5.
The influence of 2.6 pairs of H22 type life cycles
Tumor model, grouping and medication are same as above, and stop observation post administration each group mouse survival number of days, and carry out conspicuousness inspection
It tests, calculates increase in life span (ILS).ILS=(T/C-1) × 100% (T/C：Administration group mouse average Survival number of days/blank pair
According to a group mouse average Survival number of days).It the results are shown in Table 6.
3 results
Influence of the 3.1 various glossy ganoderma powder Aqueous extracts to H22 type mice with tumor tumor suppressions
Ganoderma lucidum Ultramicro-powder has apparent inhibition, and enhance with the increase of dosage to H22 growths.It is shown in Table 5.
Influence of the 3.2 various glossy ganoderma powder Aqueous extracts to mice transplanted tumor H22 type life cycles
Ganoderma lucidum Ultramicro-powder can significantly extend the life span of mouse, and increase in life span reaches as high as 86.67%.It is shown in Table 6.
Influence of the 5 each glossy ganoderma powder Aqueous extracts of table to transplanted tumor H22 type tumor suppressions
Note：Compared with physiological saline group：*：p<0.05、**：p<0.01
Influence of the 6 ganoderma lucidum Ultramicro-powder Aqueous extracts of table to transplanted tumor H22 type life cycles
Note：Compared with physiological saline group：*：p<0.05、**：p<0.01
9 ganoderma lucidum Ultramicro-powder hypoglycemic effect of embodiment
1 material
The preparation of 1.1 ganoderma lucidum Ultramicro-powder Aqueous extracts takes common flour and the ganoderma lucidum Ultramicro-powder 100g of embodiment 1,2,3 respectively, adds
Water about 1000ml impregnates 48 hours, and soak is spare to 500ml through distillation and concentration.Experimental animal uses two level SD male rats
112,210 ± 5.3g of weight.
2 methods
The foundation of diabetes rat model takes two level SD male rats 8 respectively, feeding 1W is adapted to, by 100mg/kg weight
Tail vein injection alloxan liquid under alloxan effect, by rat Langerhans islet Lu's cellular damage, causes insulin to hinder
Hinder, form experimental diabetic rats model.
After 2.1 blood sugar detection diabetes rat modeling 1W, it is randomly divided into A, two groups of B respectively, separately sets the blank pair of non-modeling
, in jejunitas 3h, blood glucose value is measured respectively, then meet AOAC Animal nutrition standards to the feeding of A, C group respectively according to 1 group of (C groups)
Basal feed, B groups feeding addition glossy ganoderma powder standard base feed, glossy ganoderma powder end content be 100ml/kg.Three groups of raising rings
Border is consistent, 25 ± 1 DEG C of temperature, relative humidity 70%.After testing 5w, tail vein is taken respectively, and blood is surveyed with ortho-aminotoluene method
Sugar value.
2.2 data processings carry out statistical procedures to the data obtained, with mean ± standard deviationIt represents, difference is shown
Work property is examined with t to be judged.
3 results
With blood sugar detection during modeling 1W the results show that A groups and C groups are substantially unchanged after feeding 5W, and the reduction of B groups blood glucose is non-
Chang Xianzhu (p<0.01), blood glucose average rate of decrease is 30.94%, and minimum blood-sugar content tends to B groups and C during normal value feeding 5W
There are significant difference (p with experimental comparison group for group blood sugar concentration<0.01) (table 7).
7 each glossy ganoderma powder of table to blood-sugar content influence (mmol/L,)
* when modeling 1W compared with：p<0.05
* is when feeding 5W compared with experimental comparison group：p<0.01
10 ganoderma lucidum Ultramicro-powder acute toxicological experiment of embodiment
Preliminary experiment：By acute toxicological experiment method, kunming mice 40 is selected, water 12h is can't help in fasting.Ultra micro ganoderma lucidum
Powder (Example 1 lot number 140918-2 and 2 lot number 140919-2 of embodiment respectively) is configured to the suspension of maximum concentration.Every
The each gavage of mouse is about 0.8mL/20g (weight), for 24 hours interior gavage 3 times, is spaced 4h.Then it routinely raises, and observes mouse
Toxic reaction situation (appearance, activity, breathing, secretion, defecation, death etc.), and continuous weighting 7 days.Because being administered with maximum
Concentration, maximum administration capacity, do not measure median lethal dose (LD50), therefore do maximum dosage-feeding experiment.
1) general performance
After administration in 14 days, the equal diet of experimental mice is normal, and fur is smooth, and freely, stool and urine is normal, without exception for activity
Secretion, respiratory system, cardiovascular system, nervous system, digestive system and urinary system are showed no exception, and mouse is all deposited
It is living.Its daily maximum dosage-feeding is that per kilogram is 180g, is equivalent to 202 times of clinical adult's dosage.
2) changes of weight situation
After administration in 14 days, weight variation without exception.
3) main organs are observed
2 groups of mouse are through gross anatomy and observe by the naked eye, and have no the abnormal phenomenon such as internal organs enlargement, atrophy, necrosis, mainly
Internal organs are close with blank control group without any bad lesion.In conclusion prompting this medicine nontoxic, clinical application amount is one
A safe dosage, clinical application safety.
Claims (8)
1. a kind of preparation method of ganoderma lucidum Ultramicro-powder obtains ganoderma lucidum average grain diameter as 100~900nm, which is characterized in that including
Following steps：
1）Using ganoderma lucidum as raw material, impurities removing is cleaned 3~5 times with drinking water, and hydraulic pressure 10MPa cuts cleaned ganoderma lucidum
Piece, then below coarse powder to 80 mesh；
2）The good ganoderma lucidum powder of coarse powder is subjected to ultra-fine grinding using the impact grinding of high energy nanometer, passes through high energy nanometer impact grinding tank body
Interior mill is situated between ceaselessly impacting 6~10 hours, and the average grain diameter of ganoderma lucidum Ultramicro-powder is made to reach 100~900nm.
2. a kind of preparation method of ganoderma lucidum Ultramicro-powder obtains ganoderma lucidum average grain diameter as 100~900nm, which is characterized in that including
Following steps：
1）Feedstock processing：Using ganoderma lucidum as raw material, it will wherein sundries reject, be cleaned 3~5 times, hydraulic pressure 10MPa with drinking water, it will be clever
Sesame is sliced；
2）Water carries：By step 1）Ganoderma lucidum be placed in extractor boil after keep boil condition 1 hour, ganoderma lucidum water is filtered to obtain in filtering
Extract and ganoderma lucidum residue, by ganoderma lucidum residue add in distilled water, after boiling keep boil condition 30min, filtering, filter ganoderma lucidum water carries
Liquid and ganoderma lucidum residue A；
3）Aqueous extracts are dried：By step 2）Ganoderma lucidum Aqueous extracts merge, be placed in Rotary Evaporators in, 60 DEG C~80 DEG C decompression rotation
It is concentrated by evaporation to dry extract, after letting cool, is put into vacuum drying chamber, 40~55 DEG C of vacuum drying obtain ganoderma lucidum water extract for 24 hours；
4）The drying of ganoderma lucidum residue and coarse powder：By step 2）Ganoderma lucidum residue A be placed at room temperature for drying, then be placed in vacuum drying chamber
Interior, 60 DEG C are dried in vacuo 24 hours, take out, put it into and coarse powder is carried out in pulverizer；
5）Ganoderma lucidum Ultramicro-powder：By step 3）Ganoderma lucidum water extract and step 4）Coarse powder merge, be put into mixing in blender, then use
Micronizer carries out ultramicro grinding to consolidated material, by mill in high energy nanometer impact grinding tank body Jie do not stop impacting 6~
10 hours, the average grain diameter of ganoderma lucidum Ultramicro-powder is made to reach 100~900nm.
3. a kind of preparation method of ganoderma lucidum Ultramicro-powder obtains ganoderma lucidum average grain diameter as 100~900nm, which is characterized in that including
Following steps：
1）Feedstock processing：Using ganoderma lucidum as raw material, it will wherein sundries reject, be cleaned 3~5 times, hydraulic pressure 10MPa with drinking water, it will be clever
Sesame is sliced；
2）Alcohol extracting：By step 1）Ganoderma lucidum add 75% ethyl alcohol, be heated to reflux 45min, filter, filter ganoderma lucidum alcohol extract and ganoderma lucidum it is residual
Ganoderma lucidum residue is added in 75% ethyl alcohol, is heated to reflux 45min, filtered, filter to obtain ganoderma lucidum alcohol extract and ganoderma lucidum residue A by slag；
3）Ganoderma lucidum alcohol extract is dried：By step 2）Ganoderma lucidum alcohol extract merge, be placed in Rotary Evaporators in, 60 DEG C~80 DEG C, subtract
Rotary evaporation is pressed, obtains ganoderma lucidum alcohol extracting thing；
4）The drying of ganoderma lucidum residue and coarse powder：By step 2）Ganoderma lucidum residue A be placed at room temperature for drying, then be placed in vacuum drying chamber
Interior, 40~55 DEG C are dried in vacuo 24 hours, take out, put it into and coarse powder is carried out in pulverizer；
5）Ganoderma lucidum Ultramicro-powder：By step 3）Ganoderma lucidum alcohol extracting thing and step 4）Coarse powder merge, be put into mixing in blender, then
Ultramicro grinding is carried out to consolidated material with micronizer, is situated between ceaselessly impacting by mill in high energy nanometer impact grinding tank body
6~10 hours, the average grain diameter of ganoderma lucidum Ultramicro-powder is made to reach 100~900nm.
4. containing the preparation method of the tablet of ganoderma lucidum Ultramicro-powder prepared by the method such as claims 1 to 3 any one, feature
It is, includes the following steps：Ganoderma lucidum Ultramicro-powder, starch, sodium carboxymethylcellulose and stearic acid are uniformly mixed, with 95% ethyl alcohol
Dissolving granulation, is put into vacuum drying chamber and is dried under vacuum to water content 3% hereinafter, then by the piece of drying and/or block for 60 DEG C
Then the particle being ground into below 14 mesh adds in magnesium stearate mixing, cross 12 mesh sieve whole grain, be pressed into plain piece, then wrap up waterproof
Film-coating.
5. containing the preparation method of the capsule of ganoderma lucidum Ultramicro-powder prepared by the method such as claims 1 to 3 any one, feature
It is, includes the following steps：30min is mixed in ganoderma lucidum Ultramicro-powder and magnesium stearate, is dissolved and pelletized with 95% ethyl alcohol, is put into
In vacuum drying chamber 60 DEG C be dried under vacuum to water content 3% hereinafter, then by the piece of drying and/or block be ground into 14 mesh with
Under particle, after 12 mesh sieve whole grain, be packed into gelatin hollow capsule, pack.
6. containing the preparation method of the particle of ganoderma lucidum Ultramicro-powder prepared by the method such as claims 1 to 3 any one, feature
It is, includes the following steps：Ganoderma lucidum Ultramicro-powder, starch, sodium carboxymethylcellulose and stearic acid are uniformly mixed, with 95% ethyl alcohol
Dissolving granulation, is put into vacuum drying chamber and is dried under vacuum to water content 3% hereinafter, then by the piece of drying and/or block for 60 DEG C
Then the particle being ground into below 14 mesh adds in magnesium stearate mixing, cross 12 mesh sieve whole grain, granule packaging.
7. ganoderma lucidum Ultramicro-powder prepared by the method such as claims 1 to 3 any one, which is characterized in that the ganoderma lucidum ultra micro
In powder, for the content of ganoderma lucidum polysaccharide not less than 0.57%, the content of ganodenic acid is not less than 1.19%.
8. ganoderma lucidum Ultramicro-powder prepared by the method such as claims 1 to 3 any one is in antitumor, hypoglycemic drug is prepared
Application.
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