CN109999129A - A kind of activity Paris polyphylla pure powder tablet preparation method - Google Patents
A kind of activity Paris polyphylla pure powder tablet preparation method Download PDFInfo
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- CN109999129A CN109999129A CN201910460116.6A CN201910460116A CN109999129A CN 109999129 A CN109999129 A CN 109999129A CN 201910460116 A CN201910460116 A CN 201910460116A CN 109999129 A CN109999129 A CN 109999129A
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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
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/896—Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
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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
- A61K9/20—Pills, tablets, discs, rods
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
- F26B5/06—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum the process involving freezing
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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
- A61K2236/31—Extraction of the material involving untreated material, e.g. fruit juice or sap obtained from fresh plants
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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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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Abstract
The invention discloses a kind of active Paris polyphylla pure powder tablet preparation methods, include the following steps: 1) to wash with water the Paris polyphylla of fresh harvesting completely, drain；2) pretreated Paris polyphylla is squeezed, collects Paris polyphylla juice and Paris polyphylla slag respectively；3) Paris polyphylla juice is concentrated under reduced pressure into the clear cream of certain relative density；4) Paris polyphylla slag is put into dryness storehouse, carries out vacuum freeze drying, dried and taken out after bleeding off pressure from dryness storehouse；5) the Paris polyphylla slag after drying is crushed with airslide disintegrating mill；6) by after Paris polyphylla juice clear cream and the mixing of Paris polyphylla ground-slag, granulation, drying, whole grain, tabletting up to active Paris polyphylla pure powder tablet.Method of the invention effectively reduces freeze-drying time, reduces energy consumption of freeze drying, improves specific yield, remains active constituent, effective component, maintains the good rehydration of product.
Description
Technical field
The present invention relates to a kind of drying means of Paris polyphylla more particularly to a kind of active Paris polyphylla pure powder tablet preparation methods.
Background technique
Paris polyphylla is the dry rhizome of liliaceous plant Yunnan Rhizoma Paridis or paris polyphylla.Also known as paris polyphylla, paris polyphylla, grass
River vehicle, is recorded in Shennong's Herbal earliest.Its bitter, cold nature is slightly poisonous, has clearing heat and detoxicating, swelling and pain relieving, cool liver fixed
The effect of frightened, for diseases such as ulcerative carbuncle, abscess of throat, venomous snake bite, injuries from falls as well, cool breeze twitch.This product hardship is let out with dropping, and trembling with fear can be clear
Heat, therefore have clearing heat and detoxicating, the function of swelling and pain relieving, to control carbuncle, swelling and furuncle, the common medicine of venomous snake bite.China's Paris polyphylla type shares 19
Kind, it is distributed mainly on southwestern each province, Yunnan is the main producing region of Paris polyphylla, there are 16 kinds to be distributed in Yunnan various regions, wherein 5 kinds are Yunnan
Area is peculiar.In recent years, it deepens continuously for the research of Paris polyphylla chemical component and its pharmacological activity, divides from the platymiscium
From identifying 50 multiple compounds such as steroid saponin, free amino acid, phytosterol, phytoecdysone, flavones.Wherein steroidal
Saponin(e is its main active, has a variety of physiological activity such as antitumor, anti-inflammatory, antibacterial, hemostasis, is clinically widely used in each
The prevention and treatment of kind cancer.
Freeze Drying Technique is much studied and is reported in the application of the dry processing of Paris polyphylla at present, it with dry, hot wind
The Paris polyphylla of seasoning production is compared, not only steroid saponin, free amino acid, phytosterol, phytoecdysone, flavones and temperature-sensitive
Property ingredient etc. is not damaged, and can keep color, nutritional ingredient, appearance and the active material of fresh goods to the maximum extent.Such as:
Number of patent application: 201310496123.4, a kind of fresh weight building ultra-fine powder preparation technology is disclosed, it is to choose fresh weight building to be washed with water
Only, impurity is removed, is drained；The microcrystalline cellulose powder of 10~20wt% of material quality is added after taking raw material fresh weight building tentatively to crush,
Then it is sufficiently mixed the raw material with the microcrystalline cellulose by the rotation of mixing machine batch can；Then material quality is added
0.7~1.3 times of water mashing；Pre-freeze after mashing, pre-freeze to be frozen into solid as standard, and maintain be frozen into solid state 5~
10 hours, pre-freezing temperature -8~-18 DEG C；The Tween 80 of 10~15wt% of grind slurries quality will be also added in the pre-freeze before pre-freeze
And it is sufficiently stirred；It is freeze-dried after pre-freeze, the control condition of freeze-drying is the time 24~120 hours at -45~-50 DEG C, together
Shi Yaoqiu moisture control is in 6wt% or less；The powder agglomates obtained after freeze-drying is pulverized into grinding kneading machine by oscillatory type
Break into micro mist.Number of patent application: 201310289915.4, the Chinese materia medica preparation Paris polyphylla disclosed for preventing and treating tumour is direct
Oral medicinal slice, it is to select fresh Paris polyphylla medicinal material, removes impurity；Ultrasonic cleaning 30min is carried out with sodium hydroxide solution；It will clean
Paris polyphylla medicinal material slice, slice thickness 1cm；Microwave drying treatment is first carried out after sliced Paris polyphylla sabot, microwave power is
400w, microwave drying total time are 1h, and freeze-drying protects 2.5h after freeze drying box temperature is down to -40 DEG C；It vacuumizes, vacuum degree
After 30Pa or less continues 5h, drying is warming up to -20 DEG C of holding 3h and is warming up to -5 DEG C of holding 5h again for the first time；It is continuously heating to
20 DEG C of holding 2h；Start redrying, be warming up to 35 DEG C, 6h is kept to terminate the drying of product when vacuum degree variation is little；It will
The dry Paris polyphylla piece completed carries out broken wall crushing under 0 DEG C of cryogenic conditions, is sieved, obtains 50-100 mesh coarse powder；It will be resulting thick
Powder continuation is crushed to 200 mesh or more under 0 DEG C of cryogenic conditions, obtains Paris polyphylla superfine powder；By gained Paris polyphylla superfine powder water system
At softwood, obtained softwood is transferred in rotary granulator, obtains 80 ~ 100 mesh particles；Particle obtained is taken, through microwave
It is aseptic subpackaged after sterilizing, finished product.
However, these vacuum freeze-drying technique sublimation dryings are all very long, energy consumption is big, and the production cycle is long, system
The about industrialized production of Freeze Drying Technique.Freeze-drying time could be saved when in some methods by being cut into very thin thickness,
But yield just declines, and specific energy consumption is increased by.Needing to be added additional auxiliary material in certain methods could be beaten, forms, be lyophilized, and increase
Add production cost, changes some original characteristics of medicinal material.
To solve drawbacks described above, there is higher cost for vacuum freeze drying, the production cycle is long, and big wait of specific energy consumption lacks
Point, inventor have carried out a large amount of research work, propose a kind of new preparation method.
Summary of the invention
Present invention aims to overcome that the shortcomings of the prior art, proposes that a kind of energy is rapidly frozen dry Paris polyphylla pure powder tablet
Method, the production cycle being entirely lyophilized is shortened, specific energy consumption and cost, which is lyophilized, to be reduced, but also sufficiently keeps fresh Paris polyphylla
Effective component, nutritional ingredient, submicron powder sheet obtained can be dissolved into rapidly molecule after adding water, and rehydration speed is fast, rehydration
Its color, quality and fresh goods are essentially identical afterwards.
To achieve the goals above, present invention employs technique below and steps:
A kind of activity Paris polyphylla pure powder tablet preparation method, it is characterised in that this method includes the following steps:
1) it by the Paris polyphylla of fresh harvesting, washes with water completely, drains；
2) pretreated Paris polyphylla is squeezed, collects Paris polyphylla juice and Paris polyphylla slag respectively；
3) the Paris polyphylla juice of step 2 is concentrated under reduced pressure into the clear cream of certain relative density；
4) the Paris polyphylla slag of step 2 is put into dryness storehouse, under the conditions of 10~50Pa of pressure, -35 DEG C~-40 DEG C of temperature, is frozen
Knot 1~2 hour；The shelf in dryness storehouse is heated again, is passed through mixed gas at the top of the dryness storehouse, control pressure is 50~
100Pa makes material rise to 0 DEG C from -35 DEG C~-40 DEG C, and lyophilization 4~6 hours, material rose to 30 DEG C from 0 DEG C, parsing-desiccation
1~2 hour, it is forced into export after normal pressure；
5) the Paris polyphylla slag after drying is subjected to 5~10min of crushing with airslide disintegrating mill at 30 DEG C or less；
It 6) will be to obtain the final product living after the mixing of the Paris polyphylla ground-slag of the Paris polyphylla juice clear cream of step 3) and step 5), granulation, drying, whole grain, tabletting
Property Paris polyphylla pure powder tablet；
7) it packs: active Paris polyphylla pure powder tablet is fitted into clean packaging, airtight vacuum or rush nitrogen and pack.
Further, reduced pressure temperature control described in step 3) is at 30~40 DEG C.
Further, the control of relative density described in step 3) is 1.1~1.3.
Further, the gas being passed through described in step 4) is the mixed gas of Krypton and neon, and mixing mass ratio is 1%~4%,
The gas temperature being passed through is controlled at 20~30 DEG C.
Further, grain size of micropowder reaches 10 μm or less after crushing described in step 5).
Further, the control of drying temperature described in step 6) is at 35~40 DEG C.
Compared with prior art, the invention has the following beneficial technical effects.
The present invention is separated juice and slag using the method for physics, is then concentrated, is lyophilized respectively etc. and operates, whole process
All it is to be handled in low temperature environment, does not destroy thermal sensitivity, active constituent and effective component.Material after freeze-drying is in loose
Porous spongy, the time and difficulty, the submicron powder sheet finally obtained for greatly reducing later period crushing can dissolve rapidly after adding water
At molecule, rehydration speed is fast, its color, quality and fresh goods are essentially identical after rehydration.
The present invention is combined using low-temperature vacuum drying and freeze-drying reasonable arrangement and effectively, and entire preparation process does not have
It is added other auxiliary materials, when granulation does not need to use additional water or alcohol as adhesive yet, to make whole preparation process unit
Total energy consumption reduce at least 50% or more, yield in unit time improve at least 50% or more, while successfully remain fresh goods color, perfume (or spice),
Taste, effective component, nutritional ingredient etc..
Drying process of the present invention both ensure that it is dry after the color of material, quality it is consistent with fresh goods, it is effective retain it is effective
Ingredient, active component content, and reduce freeze-drying time, accelerate freeze drying rate, reduces specific energy consumption, be conducive to production cost
It saves.
Product after present invention freeze-drying using vacuum or nitrogen-filled packaging and is kept in dark place, and long shelf-life is more advantageous to product
Stability during storage.
Specific embodiment
Below with reference to embodiment, the present invention is further explained, but is not intended to limit the scope of the invention.
Embodiment 1
A kind of activity Paris polyphylla pure powder tablet preparation method, method includes the following steps:
1) it by the Paris polyphylla of fresh harvesting, washes with water completely, drains；
2) pretreated Paris polyphylla is squeezed, collects Paris polyphylla juice and Paris polyphylla slag respectively；
It 3) is 30 DEG C of clear creams for being concentrated under reduced pressure into relative density and being 1.1 in temperature by the Paris polyphylla juice of step 2；
4) the Paris polyphylla slag of step 2 is put into dryness storehouse, under the conditions of 10~50Pa of pressure, -35 DEG C~-40 DEG C of temperature, is frozen
Knot 1~2 hour；The shelf in dryness storehouse is heated again, the gaseous mixture of 30 DEG C of Kryptons and neon is passed through from dryness storehouse top
Body, mixed gas mass ratio are 4%, and control pressure is 50~100Pa, so that material is risen to 0 DEG C from -35 DEG C~-40 DEG C, distillation is dry
Dry 4 hours, material rose to 30 DEG C from 0 DEG C, parsing-desiccation 2 hours, was forced into export after normal pressure；
5) the Paris polyphylla slag after drying is subjected to crushing 5min with airslide disintegrating mill at 30 DEG C or less, so that grain size of micropowder reaches 10 μm
Below；
6) the Paris polyphylla ground-slag of the Paris polyphylla juice clear cream of step 3) and step 5) is mixed, granulation, dry (temperature is controlled 35~40
DEG C), whole grain, after tabletting up to active Paris polyphylla pure powder tablet；
7) it packs: active Paris polyphylla pure powder tablet is fitted into clean packaging, airtight vacuum or rush nitrogen and pack.
Control group is set simultaneously, uses fresh Paris polyphylla and the Paris polyphylla piece of conventional furnace drying method preparation for control group.
| Title | Color | The total amount (%) (based on dry product) of I containing chonglou saponin, chonglou saponin II, chonglou saponin VI and chonglou saponin VII |
| Embodiment 1 | White | 4.63 |
| Oven drying method prepares Paris polyphylla piece | Yellow-white | 2.36 |
| Fresh Paris polyphylla | White (section) | 4.68 |
It can be seen that Paris polyphylla obtained by drying process of the present invention from above-mentioned correlation data and both maintained conventional vacuum freeze-drying
The fine quality of Paris polyphylla remains effective component, active component content, and the color of material, quality are consistent with fresh goods after drying, again
The time for shortening vacuum freeze-drying technique, freeze drying rate is accelerated, reduce specific energy consumption, increases specific yield.
Embodiment 2
A kind of activity Paris polyphylla pure powder tablet preparation method, method includes the following steps:
1) it by the Paris polyphylla of fresh harvesting, washes with water completely, drains；
2) pretreated Paris polyphylla is squeezed, collects Paris polyphylla juice and Paris polyphylla slag respectively；
It 3) is 35 DEG C of clear creams for being concentrated under reduced pressure into relative density and being 1.2 in temperature by the Paris polyphylla juice of step 2；
4) the Paris polyphylla slag of step 2 is put into dryness storehouse, under the conditions of 10~50Pa of pressure, -35 DEG C~-40 DEG C of temperature, is frozen
Knot 1~2 hour；The shelf in dryness storehouse is heated again, the gaseous mixture of 25 DEG C of Kryptons and neon is passed through from dryness storehouse top
Body, mixed gas mass ratio are 1%, and control pressure is 50~100Pa, so that material is risen to 0 DEG C from -35 DEG C~-40 DEG C, distillation is dry
Dry 5 hours, material rose to 30 DEG C from 0 DEG C, parsing-desiccation 1 hour, was forced into export after normal pressure；
5) the Paris polyphylla slag after drying is subjected to crushing 8min with airslide disintegrating mill at 30 DEG C or less, so that grain size of micropowder reaches 10 μm
Below；
6) the Paris polyphylla ground-slag of the Paris polyphylla juice clear cream of step 3) and step 5) is mixed, granulation, dry (temperature is controlled 35~40
DEG C), whole grain, after tabletting up to active Paris polyphylla pure powder tablet；
7) it packs: active Paris polyphylla pure powder tablet is fitted into clean packaging, airtight vacuum or rush nitrogen and pack.
Control group is set simultaneously, is cut into after fresh Paris polyphylla is cleaned with a thickness of 0.2cm piece, pre-freeze, distillation are then carried out
Dry, parsing-desiccation (mixed gas is not passed through in drying process), biodiversity content are crushed again after being 5% or less, are pelletized
(using water as adhesive), drying, whole grain, tabletting.
Using lyophilized technique of the invention, sublimation drying is only needed 6~7 hours, and control group sublimation drying is at least
20 hours or more are needed, freeze-drying specific energy consumption at least reduces 50% or more, and whole preparation process unit total energy consumption is also reduced to few
50% or more, yield in unit time improves at least 50% or more, while successfully remaining fresh goods color, effective component, battalion
Form point etc..
Embodiment 3
A kind of activity Paris polyphylla pure powder tablet preparation method, method includes the following steps:
1) it by the Paris polyphylla of fresh harvesting, washes with water completely, drains；
2) pretreated Paris polyphylla is squeezed, collects Paris polyphylla juice and Paris polyphylla slag respectively；
It 3) is 40 DEG C of clear creams for being concentrated under reduced pressure into relative density and being 1.3 in temperature by the Paris polyphylla juice of step 2；
4) the Paris polyphylla slag of step 2 is put into dryness storehouse, under the conditions of 10~50Pa of pressure, -35 DEG C~-40 DEG C of temperature, is frozen
Knot 1~2 hour；The shelf in dryness storehouse is heated again, the gaseous mixture of 20 DEG C of Kryptons and neon is passed through from dryness storehouse top
Body, mixed gas mass ratio are 2%, and control pressure is 50~100Pa, so that material is risen to 0 DEG C from -35 DEG C~-40 DEG C, distillation is dry
Dry 6 hours, material rose to 30 DEG C from 0 DEG C, parsing-desiccation 1 hour, was forced into export after normal pressure；
5) the Paris polyphylla slag after drying is subjected to crushing 10min with airslide disintegrating mill at 30 DEG C or less, so that grain size of micropowder reaches 10 μ
M or less；
6) the Paris polyphylla ground-slag of the Paris polyphylla juice clear cream of step 3) and step 5) is mixed, granulation, dry (temperature is controlled 35~40
DEG C), whole grain, after tabletting up to active Paris polyphylla pure powder tablet；
7) it packs: active Paris polyphylla pure powder tablet is fitted into clean packaging, airtight vacuum or rush nitrogen and pack.
Control group is set simultaneously, change 3 step 4) of embodiment use be not passed through gas, be passed through pure Krypton and pure neon for pair
According to group.
| Title | Color | Dried frozen aquatic products water content (%) |
| Embodiment 3 | White | 4.11 |
| It is not passed through gas | Ivory buff | 7.87 |
| It is passed through pure Krypton | White | 5.33 |
| It is passed through pure neon | White | 5.75 |
The result shows that can quickly reduce dried frozen aquatic products water content using the mixed inert gas of two kinds of different densities, shorten
Sublimation drying reaches drying purpose, plays a role to energy consumption of freeze drying is reduced.
Embodiment described above is used for the purpose of absolutely proving example that is of the invention and enumerating, and protection scope of the present invention is not
It is limited to this.Those skilled in the art can be modified or improve on the basis of the present invention or by a similar method
Substitution, it is within the scope of the present invention.
Claims (6)
1. a kind of activity Paris polyphylla pure powder tablet preparation method, it is characterised in that this method includes the following steps:
1) it by the Paris polyphylla of fresh harvesting, washes with water completely, drains；
2) pretreated Paris polyphylla is squeezed, collects Paris polyphylla juice and Paris polyphylla slag respectively；
3) the Paris polyphylla juice of step 2 is concentrated under reduced pressure into the clear cream of certain relative density；
4) the Paris polyphylla slag of step 2 is put into dryness storehouse, under the conditions of 10~50Pa of pressure, -35 DEG C~-40 DEG C of temperature, is frozen
Knot 1~2 hour；The shelf in dryness storehouse is heated again, is passed through mixed gas at the top of the dryness storehouse, control pressure is 50~
100Pa makes material rise to 0 DEG C from -35 DEG C~-40 DEG C, and lyophilization 4~6 hours, material rose to 30 DEG C from 0 DEG C, parsing-desiccation
1~2 hour, it is forced into export after normal pressure；
5) the Paris polyphylla slag after drying is subjected to 5~10min of crushing with airslide disintegrating mill at 30 DEG C or less；
It 6) will be to obtain the final product living after the mixing of the Paris polyphylla ground-slag of the Paris polyphylla juice clear cream of step 3) and step 5), granulation, drying, whole grain, tabletting
Property Paris polyphylla pure powder tablet；
7) it packs: active Paris polyphylla pure powder tablet is fitted into clean packaging, airtight vacuum or rush nitrogen and pack.
2. the method according to claim 1, wherein the control of reduced pressure temperature is 30~40 described in step 3)
℃。
3. the method according to claim 1, wherein the control of relative density described in step 3) is 1.1~1.3.
4. the method according to claim 1, wherein the gas being passed through described in step 4) is the mixed of Krypton and neon
Gas is closed, mixing mass ratio is 1%~4%, and the gas temperature being passed through is controlled at 20~30 DEG C.
5. the method according to claim 1, wherein described in step 5) crush after grain size of micropowder reach 10 μm with
Under.
6. the method according to claim 1, wherein the control of drying temperature described in step 6) is at 35~40 DEG C.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103393896A (en) * | 2013-07-11 | 2013-11-20 | 浙江磐谷药源有限公司 | Traditional Chinese medicine formulation paris polyphylla direct-oral decoction piece for preventing and treating tumors |
| CN103520442A (en) * | 2013-10-22 | 2014-01-22 | 浙江百草中药饮片有限公司 | Preparation technology for fresh paris polyphylla superfine powder |
| CN104906383A (en) * | 2015-05-12 | 2015-09-16 | 浙江尖峰健康科技有限公司 | Method for rapid freeze drying of active dendrobium officinale |
| CN106620156A (en) * | 2016-09-30 | 2017-05-10 | 道真仡佬族苗族自治县华毅中药材专业合作社 | Processing technology of rhizoma paridis ultrafine powder |
-
2019
- 2019-05-30 CN CN201910460116.6A patent/CN109999129A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103393896A (en) * | 2013-07-11 | 2013-11-20 | 浙江磐谷药源有限公司 | Traditional Chinese medicine formulation paris polyphylla direct-oral decoction piece for preventing and treating tumors |
| CN103520442A (en) * | 2013-10-22 | 2014-01-22 | 浙江百草中药饮片有限公司 | Preparation technology for fresh paris polyphylla superfine powder |
| CN104906383A (en) * | 2015-05-12 | 2015-09-16 | 浙江尖峰健康科技有限公司 | Method for rapid freeze drying of active dendrobium officinale |
| CN106620156A (en) * | 2016-09-30 | 2017-05-10 | 道真仡佬族苗族自治县华毅中药材专业合作社 | Processing technology of rhizoma paridis ultrafine powder |
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Application publication date: 20190712 |