CN109568272A - A kind of preparation method of ganoderma lucidum granule - Google Patents
A kind of preparation method of ganoderma lucidum granule Download PDFInfo
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- 241000222336 Ganoderma Species 0.000 claims abstract description 22
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- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 claims description 4
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- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 4
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- 229960004853 betadex Drugs 0.000 claims description 4
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- 239000008101 lactose Substances 0.000 claims description 4
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 4
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- BSEYIQDDZBVTJY-UHFFFAOYSA-N Ganoderic acid A Natural products CC(CC(=O)CCC1CC(O)C2(C)C3=C(C(=O)CC12C)C4(C)CCC(=O)C(C)(C)C4CC3O)C(=O)O BSEYIQDDZBVTJY-UHFFFAOYSA-N 0.000 description 19
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- 241001609931 bacterium 20 Species 0.000 description 3
- 230000033001 locomotion Effects 0.000 description 3
- 241000222341 Polyporaceae Species 0.000 description 2
- 241000207961 Sesamum Species 0.000 description 2
- 235000003434 Sesamum indicum Nutrition 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
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- 238000011144 upstream manufacturing Methods 0.000 description 2
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- 241001489091 Ganoderma sinense Species 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
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Classifications
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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
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1605—Excipients; Inactive ingredients
- A61K9/1629—Organic macromolecular compounds
- A61K9/1652—Polysaccharides, e.g. alginate, cellulose derivatives; Cyclodextrin
-
- 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
- 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
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
-
- 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
- A61K2236/17—Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
-
- 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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- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Medicinal Chemistry (AREA)
- Veterinary Medicine (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Chemical & Material Sciences (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Mycology (AREA)
- Animal Behavior & Ethology (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Microbiology (AREA)
- Medical Informatics (AREA)
- Botany (AREA)
- Biotechnology (AREA)
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Abstract
The invention discloses a kind of preparation methods of ganoderma lucidum granule, comprising: a, by lucid ganoderma decoction piece is carried out broken or is chopped into coarse granule；B, coarse granule is continuously inputted to Continuous Countercurrent Extraction machine, in the end of extraction pipes at different levels continues that hot water is inversely added, continuous dynamic countercurrent extracts, and collects extracting solution, and the dregs of a decoction are discharged；C, extracting solution filters, and ultra high temperature short time sterilization, filtrate decompression is condensed into clear cream；D, clear cream dissolution is added in auxiliary material, is spray-dried to obtain dry extract；E, pharmaceutical adjunct is added in dry extract, be mixed, dry granulation to obtain the final product.The present invention uses Continuous Countercurrent Extraction, high-temperature short-time sterilization, reduced pressure, spray drying, dry granulation production technology, and various process parameters are studied, to enable active constituent content in granule sustainedly and stably to reach higher level, ensure that the active constituent rate of transform and standard decoction reach the product quality for unanimously improving ganoderma lucidum granule.
Description
Technical field
The invention belongs to Chinese medicinal granule technical fields, and in particular to a kind of preparation method of ganoderma lucidum granule.
Background technique
Ganoderma lucidum is On Polyporaceae red sesame Ganoderma lucidum(leyss. ex Fr.)Or purple sesame Karst.Ganoderma sinense The drying fructification of Zhao, Xu et Zhang.Whole year harvesting, removes impurity, wipes out with rotten
The lower end stem of wood, silt or culture substrate dries in the shade or dries at 40~50 DEG C.
Chinese medicinal granule is to be mentioned, be concentrated through water by single medicinal material medicine materical crude slice, dried, pelletized, in tcm clinical practice formula
Afterwards, it takes after mixing it with water use for patient.The quality level of Chinese medicinal granule is with paste-forming rate, finger-print or characteristic spectrum, main work
Property the ingredient rate of transform (or content) three norms and standard decoction (being prepared with the preparation method of traditional Chinese medicine decoction) consistency
It is evaluated.
Chinese medicinal granule is prepared as a kind of industrialization product, production equipment, technique, process control and standard decoction
Process is there are huge difference, such as standard decoction is the low temperature concentration of short time, dry process, and Chinese medicinal granule must be through
Cross the concentration of long period under the conditions of certain temperature, it is dry could form the particle used for medical institutions' adjustment, it is different
The quality that equipment, technique and process control both make generates difference, at the same different kinds because its ingredient physics, change
It learns distinct, different tendency of changes or rule is presented in process of production.How by equipment and technological means, make industry
The product of change obtains and the consistent clinical effectiveness of traditional Chinese medicine decoction, is that Chinese medicinal granule studies most important purpose.
The existing production technology of ganoderma lucidum Chinese medicinal granule is mainly using the static extracting method decocted, most of traditional Chinese medicine extraction
The industrialization extraction process of object is all two pan-fried techniques, porous since On Polyporaceae class medicinal material is light, relatively dry, after decoction
Dregs of a decoction water swelling causes drawing liquid to slag tap difficulty, and production efficiency is low, and exists and decoct that temperature is high, decocting time is long, production efficiency
It is low, energy consumption it is at high cost, Reishi sporule active ingredient loss is more the defects of.Main active ganoderic acid A in ganoderma lucidum fruitbody
There are thermal instability when being extracted using water as solvent, decoction, the sterilizing of clear cream ingredient are proposed in water, is grown in wet granulation drying course
The influence of time high temperature is degraded, thus causes the rate of transform low, and content deviates standard decoction technical requirements range, is influenced and is faced
Bed medication is safely, effectively.
Continuous dynamic countercurrent extraction is novel extraction process in recent years, it collects extraction, weight diacolation, dynamic and adverse current skill
What art was integrated has many advantages, such as that simple process, saving solvent, low energy consumption, extraction time is short, extraction efficiency is high.Currently, not yet
See the report using continuous dynamic countercurrent water extraction process preparation ganoderma lucidum granule.
Summary of the invention
In order to overcome above-mentioned the problems of the prior art, the purpose of the present invention is to provide a kind of systems of ganoderma lucidum granule
Preparation Method, this method are raw using Continuous Countercurrent Extraction, high temperature, short time sterilizing, reduced pressure, instantaneous spray drying and dry granulation
Production. art enables active constituent content in ganoderma lucidum granule sustainedly and stably to reach higher level, it is ensured that ganoderma lucidum formula
The rate of transform of active constituent reaches ganoderma lucidum standard decoction technical requirements range in grain.
The present invention is achieved through the following technical solutions；
A kind of preparation method of ganoderma lucidum granule, includes the following steps:
A, by the pre-treatment of ganoderma lucidum medicinal material or processing, lucid ganoderma decoction piece is obtained, then carry out broken or is chopped into coarse granule；
B, the extraction pipe that the coarse granule after broken or chopping is continuously inputted to Continuous Countercurrent Extraction machine by the feed inlet of front end, is soaking
It mentions and material is continuously pushed to forward by extraction pipe slag-drip opening by a set of helical structure in pipe slags tap, in the ends of extraction pipes at different levels
Be continuously added into 10~25 times amount hot water, preferably 12~20 times amount, continuous dynamic countercurrent extract 0.5~3.0h, preferably 1~
2h, hot water and material collect extracting solution in liquid is brought out before reverse flow to extraction pipes at different levels, and the dregs of a decoction are discharged；
C, extracting solution filters, ultra high temperature short time sterilization, and filtrate is concentrated under reduced pressure into relative density as 1.00 at 55~65 DEG C~
1.10 clear cream；
D, auxiliary material dissolution is added in qinghuo reagent, is spray-dried to obtain dry extract；
E, pharmaceutical adjunct is added in dry extract, dry granulation obtains ganoderma lucidum granule.
The present invention carries out the extraction process of ganoderma lucidum using continuous dynamic countercurrent extractor, and the Continuous Countercurrent Extraction machine is
The horizontal spiral Continuous Countercurrent Extraction machine of 10 section pipe structure of stage type, compared to pot group type countercurrent extraction machine group, horizontal spiral connects
Continuous countercurrent extraction machine has agglomerated the features such as dynamic countercurrent extraction, the extruding of continuous slag charge, continuous automatic slag-liquid separation and filtering, realizes
Whole serialization, automatic control, fast low temperature extract.It extracts principle are as follows: lucid ganoderma decoction piece is continuous by feed inlet (front end)
The extraction pipe of Continuous Countercurrent Extraction machine is added, material is continuously pushed to forward by a set of helical structure by extraction in extraction pipe
Pipe slag-drip opening (end) is slagged tap, and water-soluble matchmaker then it is at different levels extraction pipes ends be continuously added into, with material in reverse flow into
Liquid is brought out before material mouth end or extraction pipe at different levels, material comes into full contact with Extraction solvent, remains the concentration gradient of solute
In higher level, so as to greatly improve the extraction rate of transform of effective component, while by controlling mentioning for extraction pipe at different levels
Take temperature, reduce the degradation of heat-sensitive ingredients at high temperature and destroy, solve drawing liquid slag tap difficulty the problems such as, it is very big to improve
Production efficiency.
The pre-treatment is to sort ganoderma lucidum medicinal material, remove impurity, obtains lucid ganoderma decoction piece.
The size of the broken partial size of raw material will affect whether effective component can be fully dissolved out, while influence extraction process object
Whether push movement is smooth forward for material, is unfavorable for solute if partial size is excessive and quickly transmits into solvent, while existing to material
Smooth retard motion in Continuous Countercurrent Extraction is easy to miss from spiral plate hole and can not be successfully transmission if partial size is too small
To slag-drip opening, it is preferred that in step a, described broken or chopping partial size is 0.3~1.0cm.
Dry lucid ganoderma decoction piece is easy to appear in blanking process to get stuck, and the wet granular after water soaks is easier blanking, from
And guarantee material can be made to come into full contact with Extraction solvent with the blanking of continuous and quantitative, while being conducive in material under effective component
Transfer is quickly extracted after material, it is preferred that in step b, lucid ganoderma decoction piece is first added to after the water wetting of 2~3 times of amounts the company of input again
In continuous dynamic countercurrent extractor.
The present invention is to extract solvent with hot water, is fed intake using hot water, and water temperature height directly affects extraction effect.Water temperature is too low
Then solvent warm-up movement is unfavorable for solute slowly and transmits into solvent water in extraction process, water temperature over-high then effective component in solvent water
Easy thermal degradation, to further illustrate influence of the water temperature height to extraction effect, water temperature is optimized in the present invention, concrete outcome
It is as follows:
| Water temperature | 25℃ | 50℃ | 75℃ | 85℃ | 95℃ | 100℃ |
| The ganoderic acid A rate of transform (%) | 28.26 | 46.18 | 52.85 | 58.17 | 51.52 | 45.38 |
If the temperature of water is lower it can be seen from the above results, it may cause effective component and extract not exclusively, if the temperature of water
Height is spent, the heat-sensitive ingredients such as ganoderic acid A are easy to happen chemical degradation in aqueous solution, it is preferred that in step b, the hot water
Temperature be 50~95 DEG C, preferably 75~95 DEG C.
Solvent amount also directly influences the extraction and degradation of active constituent, and the present invention has further carried out solvent amount excellent
Change, concrete outcome is as follows:
| Solvent amount | 8 times of amounts | 10 times of amounts | 12 times of amounts | 15 times of amounts | 20 times of amounts | 25 times of amounts |
| The ganoderic acid A rate of transform (%) | 38.64 | 44.69 | 50.99 | 56.72 | 53.26 | 48.41 |
If solvent amount is very few it can be seen from the above results, active constituent cannot reach higher in each extraction pipeline section
Concentration difference, physical transfer is incomplete, and when solvent amount reaches 15 times of amounts, the ganoderic acid A rate of transform reaches peak-peak, if solvent
Amount is excessive, and not only energy consumption improves, but also extracting solution also accordingly extends in concentration time, and ingredient is made to degrade in enriching section, from
And the rate of transform of ganoderic acid A can be reduced.Therefore, the additional amount of the hot water is 10~25 times of amounts, preferably 12~20 times amounts.
Extraction time of the material in extraction pipe is also related to the physical transfer rate and chemical degradation of active constituent, the present invention
Further extraction time to be optimized, concrete outcome is as follows:
| Extraction time | 0.5h | 1h | 2h | 3h | 4h |
| The ganoderic acid A rate of transform (%) | 46.19 | 54.31 | 60.01 | 51.45 | 45.12 |
If extraction time is short it can be seen from the above results, active constituent physical transfer is incomplete, if extraction time mistake
Long, ganoderic acid A chemical degradation rate is high, while reducing production efficiency.Preferably, in step b, lucid ganoderma decoction piece is in continuous dynamic countercurrent
Extraction time is 0.5~3.0h, preferably 1 ~ 2h in extraction.
For the rate of transform for further increasing effective component, it is preferred that in step b, by the ganoderma lucidum dregs of a decoction through squeezing recovery section
It being then exhausted from after medical fluid, the part medical fluid of recycling merges with extracting solution, so as to further increase the rate of recovery of lucidum extracting liquid,
Increase the rate of transform of effective component.
Preferably, in step b, the coarse grained input speed is 100~250kg/h, the reverse flow velocity that hot water is added
For 1000~6250kg/h.The present invention is fed by continuous and quantitative, comes into full contact with material with Extraction solvent, and the extraction of equipment is held
It is easily added, is constantly updated, so that material be made to be constantly in biggish concentration gradient throughout the extraction process with certain flow velocity
Difference is conducive to being fully dissolved out for effective component, and then can greatly improve the rate of transform of effective component in ganoderma lucidum.
Contain heat-sensitive ingredients in lucid ganoderma decoction piece, in order to avoid heat-sensitive ingredients decomposition, further increases the rate of transform, this hair
Bright first to refilter after the extracting solution cooling in step c, the present invention is further optimized cooling temperature, and concrete outcome is such as
Under:
| Cool down temperature | 30℃ | 45℃ | 55℃ | 65℃ | 75℃ |
| The ganoderic acid A rate of transform (%) | 46.89 | 52.55 | 57.59 | 56.47 | 47.13 |
The thermal degradation that can effectively avoid ganoderic acid A after extracting solution cooling it can be seen from the above results is conducive to the reservation of its content
And improve the rate of transform.When being cooled to 30~65 DEG C of temperature ranges, ganoderic acid A thermal degradation is less and tends towards stability, in combination with
The temperature that extracting solution is concentrated after cooling is excellent to reduce heating energy consumption when extracting solution concentration in 55~65 DEG C of temperature ranges
Choosing, in step c, refiltered after extracting solution is first cooled to 45~55 DEG C.
The present invention uses Continuous Countercurrent Extraction, and Extracting temperature is lower, and product microorganism risk of exceeding criterion is big, and it is further right to need
Extracting solution carries out ultra high temperature short time sterilization, to prevent ganoderic acid A from chemical degradation occurring in sterilization process, it is preferred that step c
In, the ultra high temperature short time sterilization is that filtrate sterilizes 2~30 seconds at 100~150 DEG C in supper high temperature instant sterilizer.
Ingredient is degraded in heat-sensitive ingredients material wet granulation drying course, is preferably suitable for dry granulation, to improve
Material viscosity, mobility meet granule melting requirement to adapt to dry granulation, are added in clear cream spray drying ingredient
Relevant auxiliary materials, and take a step forward in dry granulation and proper auxiliary materials are added adjust its mobility, compressibility.Preferably, in step d,
The auxiliary material is one or more of maltodextrin, dextrin, starch, lactose or beta-cyclodextrin；The technique of the spray drying
Parameter are as follows: 160 DEG C~185 DEG C of inlet air temperature, 80 DEG C~100 DEG C of leaving air temp of control.
Preferably, in step e, the pharmaceutical adjunct is maltodextrin, dextrin, starch, lactose, beta-cyclodextrin, titanium dioxide
One or more of silicon or magnesium stearate, dosage are the 0.01~0.5% of dry extract weight.
Compared with prior art, the present invention having the following beneficial effects:
(1) present invention can keep concentration difference between solute and solvent using continuous flow upstream for a long time, and can be in lower temperature
The characteristics of lower extraction, improves the physics of ganoderic acid A during the extraction process and dissolves out the rate of transform, while can carry out temperature with lower temperature
Leaching is continuous to extract, and reduces the degradation of heat-sensitive ingredients at high temperature and destroys, and solve drawing liquid slag tap difficulty the problems such as, greatly
Improve production efficiency.
(2) present invention makes microorganism be inactivated and produce under superhigh temperature in short-term using ultra high temperature short time sterilization technology (UHT)
The characteristics of product ingredient does not change prevents degradation of the ganoderic acid A in spray drying blending process, and preferably various granulations are auxiliary
Material carries out dry granulation, prevents active constituent from crossing in kind in preparation and changes.
(3) present invention combines Continuous Countercurrent Extraction, ultra high temperature short time sterilization, reduced pressure, spray drying, dry granulation raw
Production. art, and various process parameters are studied, so that lucid ganoderma decoction piece Chinese medicinal granule ganoderic acid A content be enable to continue surely
Surely reach higher level, it is ensured that the active constituent rate of transform and ganoderma lucidum standard decoction reach unanimously in granule, improve
The product quality of ganoderma lucidum granule.
Specific embodiment
Further illustrate that the present invention, following embodiment are the specific embodiment party of the present invention below by specific embodiment
Formula, but embodiments of the present invention are not limited by following embodiments.
Embodiment 1:
A kind of preparation method of ganoderma lucidum granule, includes the following steps:
A, ganoderma lucidum medicinal material is selected, shaking weeds out except impurity, obtains lucid ganoderma decoction piece, the coarse granule of 0.5cm is then broken into crusher；
B, 2 times of amount water of coarse granule are soaked, spiral Continuous Countercurrent Extraction machine (stage type is continuously inputted by the feed inlet of front end
10 section pipe structures) extraction pipe, extraction pipe in by a set of helical structure by material continuously forward push to extraction pipe deslagging
Mouth is slagged tap, and is continuously added into 16 times of 90 DEG C of hot water Continuous Countercurrent Extraction 2h in the ends of extraction pipes at different levels, hot water is with material in inverse
Liquid is brought out to flowing to before extraction pipes at different levels, extracting solution is collected, the ganoderma lucidum dregs of a decoction is then exhausted from after squeezing recovery section medical fluid,
The part medical fluid of recycling merges with extracting solution；The input speed of the lucid ganoderma decoction piece is 100kg/h, the reverse flow velocity that hot water is added
For 1600L/h；
C, the extracting solution after merging filters after being cooled to 55 DEG C, and filtered fluid goes out at 105 DEG C in supper high temperature instant sterilizer (UHT)
Bacterium 20 seconds, after at 60 DEG C be concentrated under reduced pressure at relative density be 1.04 clear cream；
D, qinghuo reagent is added maltodextrin and dissolves and stir evenly, and is spray-dried, obtains dry extract, the spray drying
Technological parameter are as follows: 160 DEG C ~ 175 DEG C of inlet air temperature, 80 DEG C ~ 90 DEG C of leaving air temp of control；
E, maltodextrin and silica is added in dry extract, is uniformly mixed, dry granulation obtains ganoderma lucidum granule.
Embodiment 2:
In step c, the extracting solution after merging does not cool down, and directly sterilizes 20 at 105 DEG C in supper high temperature instant sterilizer (UHT)
Second, after at 60 DEG C be concentrated under reduced pressure at relative density be 1.04 clear cream；
Remaining is the same as embodiment 1.
Embodiment 3:
It is in step b, coarse granule is nonwetting, spiral Continuous Countercurrent Extraction machine (stage type is continuously inputted by the feed inlet of front end
10 section pipe structures) extraction pipe, extraction pipe in by a set of helical structure by material continuously forward push to extraction pipe deslagging
Mouth is slagged tap, and is continuously added into 16 times of 90 DEG C of hot water Continuous Countercurrent Extraction 2h in the ends of extraction pipes at different levels, hot water is with material in inverse
Liquid is brought out to flowing to before extraction pipes at different levels, collects extracting solution；The ganoderma lucidum dregs of a decoction are discharged；The input speed of the lucid ganoderma decoction piece
For 100kg/h, the reverse flow velocity that hot water is added is 1600L/h；
Remaining is the same as embodiment 1.
Embodiment 4:
A kind of preparation method of ganoderma lucidum granule, includes the following steps:
A, ganoderma lucidum medicinal material is selected, shaking weeds out except impurity, obtains lucid ganoderma decoction piece, be then broken into 0.5cm coarse granule with crusher；
B, 3 times of amount water of coarse granule are soaked, spiral Continuous Countercurrent Extraction machine (stage type is continuously inputted by the feed inlet of front end
10 section pipe structures) extraction pipe, extraction pipe in by a set of helical structure by material continuously forward push to extraction pipe deslagging
Mouth is slagged tap, and is continuously added into 18 times of 85 DEG C of hot water Continuous Countercurrent Extraction 1.5h in the ends of extraction pipes at different levels, hot water is with material in inverse
Liquid is brought out to flowing to before extraction pipes at different levels, extracting solution is collected, the ganoderma lucidum dregs of a decoction is then exhausted from after squeezing recovery section medical fluid,
The part medical fluid of recycling merges with extracting solution；The input speed of the lucid ganoderma decoction piece is 100kg/h, the reverse flow velocity that hot water is added
For 1800L/h；
C, the extracting solution after merging filters after being cooled to 50 DEG C, and filtered fluid goes out at 150 DEG C in supper high temperature instant sterilizer (UHT)
Bacterium 10 seconds, after at 65 DEG C be concentrated under reduced pressure at relative density be 1.04 clear cream；
D, qinghuo reagent is added maltodextrin and dissolves and stir evenly, and is spray-dried, obtains dry extract, the spray drying
Technological parameter are as follows: 175 DEG C ~ 185 DEG C of inlet air temperature, 90 DEG C ~ 100 DEG C of leaving air temp of control；
E, maltodextrin and silica is added in dry extract, is uniformly mixed, dry granulation obtains ganoderma lucidum granule.
Embodiment 5:
A kind of preparation method of ganoderma lucidum granule, includes the following steps:
A, ganoderma lucidum medicinal material is selected, shaking weeds out except impurity, obtains lucid ganoderma decoction piece, the coarse granule of 0.5cm is then broken into crusher；
B, 2 times of amount water of coarse granule are soaked, spiral Continuous Countercurrent Extraction machine (stage type is continuously inputted by the feed inlet of front end
10 section pipe structures) extraction pipe, extraction pipe in by a set of helical structure by material continuously forward push to extraction pipe deslagging
Mouth is slagged tap, and is continuously added into 20 times of 75 DEG C of hot water Continuous Countercurrent Extraction 1.5h in the ends of extraction pipes at different levels, hot water is with material in inverse
Liquid is brought out to flowing to before extraction pipes at different levels, extracting solution is collected, the ganoderma lucidum dregs of a decoction is then exhausted from after squeezing recovery section medical fluid,
The part medical fluid of recycling merges with extracting solution；The input speed of the lucid ganoderma decoction piece is 60kg/h, the reverse flow velocity that hot water is added
For 1200L/h；
C, the extracting solution after merging filters after being cooled to 45 DEG C, and filtered fluid goes out at 105 DEG C in supper high temperature instant sterilizer (UHT)
Bacterium 20 seconds, after at 60 DEG C be concentrated under reduced pressure at relative density be 1.04 clear cream；
D, qinghuo reagent is added maltodextrin and dissolves and stir evenly, and is spray-dried, obtains dry extract, the spray drying
Technological parameter are as follows: 175 DEG C ~ 185 DEG C of inlet air temperature, 90 DEG C ~ 100 DEG C of leaving air temp of control；
E, maltodextrin and silica is added in dry extract, is uniformly mixed, dry granulation obtains ganoderma lucidum granule.
Comparative example 1: Chinese medicine extracting tank is used
A kind of preparation method of ganoderma lucidum granule, includes the following steps:
A, ganoderma lucidum medicinal material is selected, shaking weeds out except impurity, obtains lucid ganoderma decoction piece, the coarse granule of 0.5cm is then broken into crusher；
B, lucid ganoderma decoction piece is added in Chinese medicine extracting tank, with water boiling and extraction 2 times, for the first time plus the water of 9 times of amounts is heated and decocted
1.0h, the water heating of second plus 7 times amount decoct 1.0h, extracting solution filtration；
C, the clear cream that relative density is 1.04 when filtrate decompression is condensed into 60 DEG C；
D, qinghuo reagent is added maltodextrin and dissolves and stir evenly, and is spray-dried, obtains dry extract, the spray drying
Technological parameter are as follows: 160 DEG C ~ 175 DEG C of inlet air temperature, 80 DEG C ~ 90 DEG C of leaving air temp of control；
E, dry extract adds maltodextrin and silica, is uniformly mixed, dry granulation obtains ganoderma lucidum granule.
Comparative example 2: pot group type countercurrent extraction machine is used
A kind of preparation method of ganoderma lucidum granule, includes the following steps:
A, ganoderma lucidum medicinal material is selected, shaking weeds out except impurity, obtains lucid ganoderma decoction piece, the coarse granule of 0.5cm is then broken into crusher；
B, medicine materical crude slice is put into the series connection extractor group formed with 5 end to end extractors by the following arrangement mode that feeds intake,
Fresh solvent is added with material-water ratio 1:16 ratio in tail tank, is extracted with 90 DEG C of each tank Extracting temperature, extraction time 2.0h:
Material in 5 tanks be successively new medicine materical crude slice, through 1 time extract after the dregs of a decoction, through 2 times extract the dregs of a decoction, through 3 times extract the dregs of a decoction,
Fresh solvent is added in (dregs of a decoction after extracting equipped with the 4th) tank of most end, other each tanks by the dregs of a decoction extracted through 4 times
It is sequentially arranged with from the extracting solution that next stage tank transfer moves past and extracts, final extracting solution is discharged from the tank of foremost, most
Extractor afterwards is discharged the dregs of a decoction and is packed into new medicine materical crude slice, becomes most preceding extractor, and so circulation is reverse extracts, collection extracting solution filter
Cross merging；
C, the extracting solution after merging filters after being cooled to 55 DEG C, and filtered fluid goes out at 105 DEG C in supper high temperature instant sterilizer (UHT)
Bacterium 20 seconds, after at 60 DEG C be concentrated under reduced pressure at relative density be 1.04 clear cream；
D, qinghuo reagent is added maltodextrin and dissolves and stir evenly, and is spray-dried, obtains dry extract, the spray drying
Technological parameter are as follows: 160 DEG C ~ 175 DEG C of inlet air temperature, 80 DEG C ~ 90 DEG C of leaving air temp of control；
E, maltodextrin and silica is added in dry extract, is uniformly mixed, dry granulation obtains ganoderma lucidum granule.
The ganoderma lucidum granule that embodiment and comparative example is prepared measures ganoderic acid A content, calculates paste-forming rate, turns
Shifting rate situation, the results are shown in Table 1:
1 ganoderma lucidum granule embodiment of table is compared with comparative example result
By embodiment 1 it is found that the present invention is mentioned using Continuous Countercurrent Extraction technology with traditional extraction tank compared with 1 result of comparative example
Take technology to compare, not only solvent consumption amount is few, but also can continuous slag charge squeeze, continuous automatic slag-liquid separation, realize it is whole even
Continuousization, automatic control, fast low temperature extract, and remain heat-sensitive ingredients ganoderic acid A content, hence it is evident that improve the rate of transform, show
The present invention is substantially better than common extractor extractive technique currently on the market using Continuous Countercurrent Extraction technology.
By embodiment 1 compared with 2 result of comparative example it is found that compared with pot group type countercurrent extraction machine, the continuous flow upstream of use
Extractive technique either paste-forming rate or heat-sensitive ingredients ganoderic acid A content and the rate of transform increase, i.e., the present invention uses
Continuous Countercurrent Extraction technology is better than pot group type countercurrent extraction machine.
By embodiment 1, it is found that the present invention is used, by extracting solution, cooling is handled rapidly compared with 2 result of embodiment, can be kept away
Exempt from the degradation of heat-sensitive ingredients, hence it is evident that improve the rate of transform of the ingredient.
By 2 ~ 5 result of embodiment it is found that the present invention, which carries out low-temperature dynamic adverse current using Continuous Countercurrent Extraction technology, extracts energy
Heat-sensitive ingredients ganoderic acid A content and the rate of transform are significantly improved, and then improves the quality of product.Meanwhile continuous dynamic countercurrent skill
Art can be further reduced the consumption of solvent in the case where guaranteeing paste-forming rate, component content and the rate of transform, be the one of economical and energy saving
The novel extracting mode of kind.
By embodiment 1 ~ 5 it is found that the present invention carries out extracting solution using ultra high temperature short time sterilization technology compared with comparative example 1
Sterilizing preferably can control microorganism from source, guarantee that the microorganism of finished product is qualified.
Claims (10)
1. a kind of preparation method of ganoderma lucidum granule, which comprises the steps of:
A, by the pre-treatment of ganoderma lucidum medicinal material or processing, lucid ganoderma decoction piece is obtained, then carry out broken or is chopped into coarse granule；
B, the extraction pipe that the coarse granule after broken or chopping is continuously inputted to Continuous Countercurrent Extraction machine by the feed inlet of front end, is soaking
It mentions and material is continuously pushed to forward by extraction pipe slag-drip opening by a set of helical structure in pipe slags tap, in the ends of extraction pipes at different levels
Be continuously added into 10~25 times amount hot water, preferably 12~20 times amount, continuous dynamic countercurrent extract 0.5~3.0h, preferably 1~
2h, hot water and material collect extracting solution in liquid is brought out before reverse flow to extraction pipes at different levels, and the dregs of a decoction are discharged；
C, extracting solution filters, ultra high temperature short time sterilization, and it is 1.00~1.10 that filtrate, which is concentrated under reduced pressure into relative density at 55-65 DEG C,
Clear cream；
D, auxiliary material dissolution is added in qinghuo reagent, is spray-dried to obtain dry extract；
E, pharmaceutical adjunct is added in dry extract, dry granulation obtains ganoderma lucidum granule.
2. the preparation method of ganoderma lucidum granule according to claim 1, which is characterized in that in step a, the pre-treatment
It is that ganoderma lucidum medicinal material is sorted, removes impurity, obtains lucid ganoderma decoction piece；Described broken or chopping partial size is 0.3~1.0cm.
3. the preparation method of ganoderma lucidum granule according to claim 1, which is characterized in that in step b, by lucid ganoderma decoction piece
It is inputted in continuous dynamic countercurrent extractor again after the water wetting of 2~3 times of amounts is first added.
4. the preparation method of ganoderma lucidum granule according to claim 1, which is characterized in that described continuous inverse in step b
Stream extractor is spiral Continuous Countercurrent Extraction machine, is 10 section pipe structure of stage type.
5. the preparation method of ganoderma lucidum granule according to claim 1, which is characterized in that in step b, the hot water
Temperature is 50~95 DEG C, preferably 75~95 DEG C.
6. the preparation method of ganoderma lucidum granule according to claim 1, which is characterized in that in step b, by the dregs of a decoction through squeezing
It is then exhausted from after pushing back receiving portions medical fluid, the part medical fluid of recycling merges with extracting solution.
7. the preparation method of ganoderma lucidum granule according to claim 1, which is characterized in that in step b, the coarse granule
Input speed be 100~250kg/h, the reverse flow velocity that hot water is added is 1000~6250kg/h.
8. the preparation method of ganoderma lucidum granule according to claim 1, which is characterized in that in step c, first by extracting solution
It is refiltered after being cooled to 45~55 DEG C；The ultra high temperature short time sterilization be by filtrate 100~150 in supper high temperature instant sterilizer
It sterilizes 2~30 seconds at DEG C.
9. the preparation method of ganoderma lucidum granule according to claim 1, which is characterized in that in step d, the auxiliary material is
One or more of maltodextrin, dextrin, starch, lactose or beta-cyclodextrin；The technological parameter of the spray drying are as follows: control
160 DEG C~185 DEG C of inlet air temperature, 80 DEG C~100 DEG C of leaving air temp.
10. the preparation method of ganoderma lucidum granule according to claim 1, which is characterized in that in step e, the preparation
Auxiliary material is the mixed of one or more of maltodextrin, dextrin, starch, lactose, beta-cyclodextrin, silica or magnesium stearate
It closes, dosage is the 0.01~0.5% of dry extract weight.
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| CN110523342A (en) * | 2019-09-30 | 2019-12-03 | 广东一方制药有限公司 | Chinese medicinal granule production equipment and method |
| CN112021555A (en) * | 2020-08-31 | 2020-12-04 | 山东省农业科学院农产品研究所 | Ganoderma lucidum spore powder tablet and preparation method thereof |
| CN110523342B (en) * | 2019-09-30 | 2024-07-09 | 广东一方制药有限公司 | Equipment and method for producing traditional Chinese medicine formula granules |
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| CN110447889A (en) * | 2019-08-23 | 2019-11-15 | 广州白云山汉方现代药业有限公司 | A kind of preparation method of Ganodenna Lucidum P.E |
| CN110523342A (en) * | 2019-09-30 | 2019-12-03 | 广东一方制药有限公司 | Chinese medicinal granule production equipment and method |
| CN110523342B (en) * | 2019-09-30 | 2024-07-09 | 广东一方制药有限公司 | Equipment and method for producing traditional Chinese medicine formula granules |
| CN112021555A (en) * | 2020-08-31 | 2020-12-04 | 山东省农业科学院农产品研究所 | Ganoderma lucidum spore powder tablet and preparation method thereof |
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