CN106389776A - Tropaeolum granule and preparation method thereof - Google Patents
Tropaeolum granule and preparation method thereof Download PDFInfo
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- CN106389776A CN106389776A CN201611071332.4A CN201611071332A CN106389776A CN 106389776 A CN106389776 A CN 106389776A CN 201611071332 A CN201611071332 A CN 201611071332A CN 106389776 A CN106389776 A CN 106389776A
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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)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/28—Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
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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)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
- A61K36/484—Glycyrrhiza (licorice)
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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)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/71—Ranunculaceae (Buttercup family), e.g. larkspur, hepatica, hydrastis, columbine or goldenseal
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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)
- A61K36/894—Dioscoreaceae (Yam family)
- A61K36/8945—Dioscorea, e.g. yam, Chinese yam or water yam
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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
- A61K9/1617—Organic compounds, e.g. phospholipids, fats
- A61K9/1623—Sugars or sugar alcohols, e.g. lactose; Derivatives thereof; Homeopathic globules
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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
- A61K9/1635—Organic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyvinyl pyrrolidone, poly(meth)acrylates
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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
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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
- A61K9/1664—Compounds of unknown constitution, e.g. material from plants or animals
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—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
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- 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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- 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
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
Abstract
The invention belongs to the field of traditional Chinese medicine preparations, and particularly relates to a tropaeolum granule and a preparation method thereof. The tropaeolum granule is prepared from the following raw materials in parts by weight: 10-20 parts of tropaeolum, 3-8 parts of crowndaisy chrysanthemum, 3-5 parts of sweet potato stem and leaf superfine powder, 1-10 parts of licorice root, 1-3 parts of xylitol and 18-45 parts of mixed auxiliary material, wherein the mixed auxiliary material is composed of dextrin, 0.5-3% (w/w) PVP alcoholic solution and corn cob superfine powder according to a weight ratio of 1 to (0.5-0.8) to (0.05-0.1). The granule has the advantages of favorable formability, low moisture absorption possibility, high stability, favorable dissolubility and high dissolution rate, and achieves an obvious effect in treatment of inappetence, heavy sensation and asthenia caused by pathogenic cold invasion, damp heat or the like; and the total effective rate is up to 100%.
Description
Technical field
The invention belongs to field of traditional Chinese is and in particular to a kind of trollius chinensis granular agent and preparation method thereof.
Background technology
Flos Trollii is dried flower for the plant Flos Trollii of Ranunculaceae Trollius, has functions that heat-clearing and toxic substances removing,
It is made into tablet, injectable powder, capsule, oral liquor and other types of formulations, be clinically used for acute and chronic tonsillitis, acute middle ear
The infectious disease such as inflammation, acute myringitis, acute conjunctivitiss, acute lymphangitiss, upper respiratory tract infection, pharyngitis.
Sweet potato genus Convolvulaceae sweet potato genus, are commonly called as Radix Ipomoeae, sweet potato, Ipomoea batatas Lam., yam etc., originate in America Mexico, and about 16
The incoming China of middle of century, has very high nutritive value.At present, both at home and abroad to sweet potato root tuber and its product developmental research very
Many, and the exploitation of the analysis and research to sweet potato leaves and stemses and its food or medicine is just at the early-stage.Sweet potato leaves and stemses contain various active
Composition, away from Asia Vegetable Research Institute centre of development report, every 100g fresh sweet potato stem and leaf 3.56g containing crude protein, crude fibre
4.10g, crude fat 0.67g, calcium 81.2mg, phosphorus 67.3mg, carotene 3.61mg, VC 25.0mg, nicotinic acid 0.94mg.It is not only
Nutritious, but also there is higher medical value.
Caulis et Folium Chrysanthemi segeti be feverfew Caulis et Folium Chrysanthemi segeti stem and leaf, warm in nature, sweet-puckery flavor, enter liver and kidney channel, purify the blood, nourishing heart, blood pressure lowering, lung moistening,
Effect of clearing away phlegm.
Radix Glycyrrhizae is the dry root of glycyrrhizic legume, Glycyrrhiza inflata Bat. or Glycyrrhiza glabra L.;Nature and flavor are sweet, flat;Invigorating the spleen and replenishing QI, heat clearing away
Removing toxic substances, expelling phlegm for arresting cough, relieving spasm to stop pain, coordinating the actions of various ingredients in a prescription.
At present, be yet there are no with Flos Trollii, sweet potato leaves and stemses superfine powder, the Caulis et Folium Chrysanthemi segeti and Radix Glycyrrhizae preparation as principle active component
Report.
Because granule has a taking convenience, the advantages of absorb fast, effective rapid, market occurs in that various gold
Flos Nelumbinis granule.As awl mountain board trollius chinensis granular, its main component is Flos Trollii, has functions that heat-clearing and toxic substances removing.
Chinese patent application 201110122227.X discloses a kind of gold with heat-clearing and toxic substances removing antibacterial and resisting virus, eliminating inflammation
Flos Nelumbinis granular preparation, is made up of following Chinese crude drugs by weight:1~100 part of Flos Trollii, 100~1 parts of Radix Scutellariae.This invention
Compound Chinese medicinal preparation has good antibacterial, resisting virus, eliminating inflammation effect, make carry taking convenience, absorb faster, instant effect
Granule, is conducive to its large-scale production.But because traditional Chinese medicine thick paste moisture content itself is more, it is difficult in actual production and pastes
Smart mix homogeneously, easily forms caking, and the granule of the Chinese medicine class easily moisture absorption itself, and this granule is also added into substantial amounts of sugarcane
Sugar, has been further exacerbated by the hygroscopicity of granule, its obtained granule less stable, easily gets damp again, is unfavorable for granule
Preserve.
Therefore, for technical problem present in above-mentioned prior art it is necessary to provide a kind of stable system it is easy to prepare
Trollius chinensis granular agent with molding.
Content of the invention
In order to solve technical problem present in prior art, it is an object of the invention to provide a kind of trollius chinensis granular agent
And preparation method thereof, to solve disadvantages described above.
The invention provides a kind of trollius chinensis granular agent, including the preparing raw material of following parts by weight:Flos Trollii 10~20
Part, 3~8 parts of Caulis et Folium Chrysanthemi segeti, 3~5 parts of sweet potato leaves and stemses superfine powder, 1~10 part of Radix Glycyrrhizae, 1~3 part of xylitol and mixed accessories 18~45
Part, wherein, described mixed accessories press 1 by dextrin, the PVP alcoholic solution of 0.5~3% (W/W) and corn cob superfine powder:(0.5~
0.8):The weight of (0.05~0.1) is than composition.
Preferably, described trollius chinensis granular agent includes the preparing raw material of following parts by weight:15 parts of Flos Trollii, Caulis et Folium Chrysanthemi segeti 6
Part, 4 parts of sweet potato leaves and stemses superfine powder, 5 parts of Radix Glycyrrhizae, 2 parts of xylitol and 26 parts of mixed accessories, wherein, described mixed accessories are by pasting
Essence, the PVP alcoholic solution of 2% (W/W) and corn cob superfine powder press 1:0.6:0.06 weight is than composition.
Preferably, described trollius chinensis granular agent includes the preparing raw material of following parts by weight:10 parts of Flos Trollii, Caulis et Folium Chrysanthemi segeti 3
Part, 3 parts of sweet potato leaves and stemses superfine powder, 1 part of Radix Glycyrrhizae, 1 part of xylitol and 18 parts of mixed accessories, wherein, described mixed accessories are by pasting
Essence, the PVP alcoholic solution of 0.5% (W/W) and corn cob superfine powder press 1:0.5:0.05 weight is than composition.
Preferably, described trollius chinensis granular agent includes the preparing raw material of following parts by weight:20 parts of Flos Trollii, Caulis et Folium Chrysanthemi segeti 8
Part, 5 parts of sweet potato leaves and stemses superfine powder, 10 parts of Radix Glycyrrhizae, 3 parts of xylitol and 45 parts of mixed accessories, wherein, described mixed accessories are by pasting
Essence, the PVP alcoholic solution of 3% (W/W) and corn cob superfine powder press 1:0.8:0.1 weight is than composition.
Preferably, described sweet potato leaves and stemses superfine powder is obtained by following steps:
Take fresh sweet potato stem and leaf, decontamination, clean, dry, be dried, broken through super micron mill after precomminution to 30~50 mesh
The powder body becoming particle diameter to be 20~50 μm, obtains final product.
Preferably, described corn cob superfine powder is obtained by following steps:
Take the corn cob after drying, chopping, being broken into particle diameter through super micron mill after precomminution to 30~50 mesh is 32~45 μ
The powder body of m, obtains final product.
Preferably, described granule also includes 0.1~0.3 part of magnesium laurylsulfate.
Correspondingly, present invention also offers a kind of method preparing above-mentioned trollius chinensis granular agent, comprise the following steps:
A) the preparation of raw material fine powder:The preparation of described raw material fine powder includes tetra- steps of S1~S4:
S1, depletion Flos Nelumbinis, Caulis et Folium Chrysanthemi segeti and Radix Glycyrrhizae, clean, dry, and are ground into 60~70 mesh, add the steaming of medical material 3~6 times amount
Distilled water decoct 1~3 time, filter, merge decoction liquor, by decoction liquor evaporation and concentration at 80~90 DEG C relative density be 1.05~
1.10 concentrated solution I, cooling, standby;
S2, be slowly added dropwise while stirring toward in above-mentioned concentrated solution I described concentrated solution I 1~2 times amount 50~60% ethanol
Solution carries out a precipitate with ethanol, takes supernatant after standing overnight, and precipitate is washed with 50~60% ethanol solution, cleaning mixture with upper
Clear liquid merges to obtain filtrate I, decompression recycling ethanol;
S3, by filtrate I again evaporation and concentration relative density at 80~90 DEG C be 1.15~1.25 concentrated solution II, add
The ethanol solution of the 80~90% of concentrated solution II 2~3 times amount carries out secondary precipitate with ethanol, takes supernatant after standing overnight, and precipitate is used
80~90% ethanol solution washing, cleaning mixture merges to obtain filtrate II, decompression recycling ethanol with supernatant;
S4, filtrate II is concentrated into the thick paste that relative density at 80~90 DEG C is 1.30~1.35, by above-mentioned thick paste through spray
Mist is dried to extract powder, adds sweet potato leaves and stemses superfine powder, mix homogeneously, obtains raw material fine powder;
B) toward in above-mentioned raw material fine powder, add xylitol, the PVP alcoholic solution of 0.5~3% (W/W) and mixed accessories, mix,
It is pressed into thick piece in advance, pulverize, sieve, obtain final product.
Preferably, described step A) described in sweet potato leaves and stemses superfine powder be obtained by following steps:
Take fresh sweet potato stem and leaf, decontamination, clean, dry, be dried, broken through super micron mill after precomminution to 30~50 mesh
The powder body becoming particle diameter to be 20~50 μm, obtains final product.
Preferably, described step B) described in mixed accessories by dextrin, the PVP alcoholic solution of 0.5~3% (W/W) and Semen Maydiss
Core superfine powder presses 1:(0.5~0.8):The weight of (0.05~0.1) is than composition.
Preferably, described step B) described in mixed accessories by dextrin, the PVP alcoholic solution of 0.5~3% (W/W) and Semen Maydiss
Core superfine powder presses 1:0.6:0.06 weight is than composition.
Preferably, described step B) also include adding 0.1~0.3 part of magnesium laurylsulfate toward in described raw material fine powder.
In granule of the present invention, Flos Trollii, Caulis et Folium Chrysanthemi segeti, sweet potato leaves and stemses superfine powder and Radix Glycyrrhizae are main Chinese medicine ingredients, its
In, Flos Trollii is preferably Yunnan globeflower, and it is warm in nature, sweet in the mouth is pungent, has heat-clearing and toxic substances removing, expelling wind and cold, induces sweat, and disappear the work(such as knot
Effect;Sweet potato leaves and stemses superfine powder is obtained through micronizing by sweet potato leaves and stemses, and compared with sweet potato stem-leaf extract, it intactly remains
Most of effective ingredient of sweet potato leaves and stemses, and its superfine powder state advantageously reduces the viscosity of traditional Chinese medicine thick paste, shortens subsequent spray
Drying time, improve production efficiency.In formula, each group is divided and is complemented each other, play altogether cold expelling and in, clearing heat and expelling damp, dispersing the stagnated liver-QI for regulating the stomach etc.
Effect, is invaded by cold-evil for treatment or the inappetence causing such as damp and hot, and the weak symptom of heavy sensation of the body has significant effect.
Inventor finds to be individually added into the prepared grain forming of dextrin typically in process of the test, and easy to stick between granule
Even, in later stage storage, easily the moisture absorption is lumpd, and storage life is shorter;PVP has good dissolubility and stability, and inventor attempts
Add PVP alcoholic solution on the basis of adding dextrin, the mouldability of the granule obtained by result is obviously improved;But inventor is same
Mono- problem of Shi Faxian, the repeatability of granule is poor, and between the granule obtained by PVP alcoholic solution of variable concentrations, properties of product are poor
Different larger, inventor, by substantial amounts of test, finally determines the particle effect obtained by PVP alcoholic solution of 0.5~3% (W/W)
Best.
But, due to the Chinese medical concrete easily moisture absorption itself, add dextrin and granule that PVP alcoholic solution is obtained also have easy suction
Wet, the problem of stability difference, it is embodied in, add dextrin and its long storage life of granule of PVP alcoholic solution is only 12
Individual month, occurred in that moisture absorption caking phenomenon at 12nd month.Inventor passes through test long-term in a large number, finally finds, above-mentioned
On the basis of add the hygroscopicity that corn cob superfine powder can dramatically improve granule, and the grain dissolution speed being obtained is fast, molten
After solution, no precipitation produces, and this point is that inventor is unexpected.Simultaneously inventor it was also found that the particle diameter of corn cob superfine powder and
Consumption has large effect to its effect.Finally, inventor is drawn by unremitting effort, by the size controlling of Semen Maydiss superfine powder
At 32~45 μm, and control its proportion with dextrin 1:The hygroscopicity of granule can greatly be improved between 0.05, and improve
The stripping property of granule.
In the present invention, Flos Trollii taste is partially bitter, adds the mouthfeel that xylitol improves granule.
The method typically adopting water boiling and precipitation with ethanol in prior art extracts Chinese medicine extract, and the method has processing ease, accurate
Exactness is high, advantage with low cost, but also has many reports to point out that precipitate with ethanol process, while removing impurity, is often lost larger
The effective ingredient of amount.Inventor find, before second precipitate with ethanol first by concentration of liquid medicine to certain concentration, can significantly reduce
The loss of effect composition.Effect test proves, compared with existing water boiling and precipitation with ethanol method, is obtained by extracting through the method for the invention
The granule obtained by Chinese medicine extraction liquid treatment is invaded by cold-evil or the inappetence causing such as damp and hot, the weak symptom of heavy sensation of the body
There is more significant effect.
Inventor finds in pelletization, when mixing extractum and adjuvant, still suffers from a little granules and reunites together.
In order to solve this problem, inventor has attempted multiple methods, finds at last, before mix extractum with adjuvant, first will soak
The spray-dried powdering of cream, then mix with adjuvant, easily by both mix homogeneously, and soilless sticking phenomenon.Magnesium laurylsulfate
It can be avoided that producing more fine powder in pelletization.
Compared with prior art, granule of the present invention has following advantage:
1) granule of the present invention has good moldability, is difficult moisture absorption, and stability is high, and it is excellent that stripping property is good and dissolution velocity is fast
Point.
2) granule of the present invention is used for treatment and is invaded by cold-evil or the inappetence causing such as damp and hot, and the weak symptom of heavy sensation of the body has
There is significant effect, total effective rate is up to 100%.
Specific embodiment:
Below by way of the description of specific embodiment, the invention will be further described, but this is not the limit to the present invention
System, according to the basic thought of the present invention, various modifications may be made or improves for those skilled in the art, but without departing from this
The basic thought of invention, all within the scope of the present invention.
Embodiment 1, the preparation of sweet potato leaves and stemses superfine powder
Take fresh sweet potato stem and leaf, decontamination, clean, dry, be dried, after precomminution to 40 mesh, be broken into grain through super micron mill
Footpath is 30 μm of powder body, obtains final product.
Embodiment 2, the preparation of corn cob superfine powder
Described corn cob superfine powder is obtained by following steps:
Take the corn cob after drying, chopping, it is broken into, through super micron mill, the powder body that particle diameter is 38 μm after precomminution to 40 mesh,
Obtain final product.
Embodiment 3, the preparation of corn cob superfine powder
Described corn cob superfine powder is obtained by following steps:
Take the corn cob after drying, chopping, it is broken into, through super micron mill, the powder body that particle diameter is 32 μm after precomminution to 30 mesh,
Obtain final product.
Embodiment 4, the preparation of corn cob superfine powder
Described corn cob superfine powder is obtained by following steps:
Take the corn cob after drying, chopping, it is broken into, through super micron mill, the powder body that particle diameter is 45 μm after precomminution to 50 mesh,
Obtain final product.
Embodiment 5, a kind of trollius chinensis granular agent
Described in the embodiment of the present invention 5, trollius chinensis granular agent is prepared from by the preparing raw material of following parts by weight:Flos Trollii
15 parts, 6 parts of Caulis et Folium Chrysanthemi segeti, 4 parts of sweet potato leaves and stemses superfine powder described in embodiment 1,5 parts of Radix Glycyrrhizae, 2 parts of xylitol and mixed accessories 26
Part, wherein, described mixed accessories press 1 by dextrin, the PVP alcoholic solution of 2% (W/W) and corn cob superfine powder described in embodiment 2:
0.6:0.06 weight is than composition.
Preparation method:
A) the preparation of raw material fine powder:The preparation of described raw material fine powder includes tetra- steps of S1~S4:
S1, depletion Flos Nelumbinis, Caulis et Folium Chrysanthemi segeti and Radix Glycyrrhizae, clean, dry, and are ground into 70 mesh, add the distilled water of medical material 5 times amount to decoct
3 times, filter, merge decoction liquor, relative density is 1.10 concentrated solution I at 85 DEG C by decoction liquor evaporation and concentration, cooling, standby
With;
S2,55% ethanol solution being slowly added dropwise described concentrated solution I 2 times amount toward in above-mentioned concentrated solution I while stirring enter
Precipitate with ethanol of row, takes supernatant, precipitate is washed with 55% ethanol solution, and cleaning mixture is merged with supernatant after standing overnight
Filtrate I, decompression recycling ethanol;
S3, by filtrate I again evaporation and concentration relative density at 85 DEG C be 1.20 concentrated solution II, add concentrated solution II 2
The ethanol solution of the 85% of times amount carries out secondary precipitate with ethanol, takes supernatant after standing overnight, and precipitate is washed with 85% ethanol solution
Wash, cleaning mixture merges to obtain filtrate II, decompression recycling ethanol with supernatant;
S4, filtrate II is concentrated into the thick paste that relative density at 85 DEG C is 1.32, by spray-dried for above-mentioned thick paste become leaching
Cream powder, adds sweet potato leaves and stemses superfine powder, mix homogeneously, obtains raw material fine powder;
B) toward in above-mentioned raw material fine powder, add xylitol, the PVP alcoholic solution of 2% (W/W) and mixed accessories, mix, precompressed
Become thick piece, pulverize, sieve, by 10g/ bag subpackage, obtain final product.
Embodiment 6, a kind of trollius chinensis granular agent
Described in the embodiment of the present invention 6, trollius chinensis granular agent is prepared from by the preparing raw material of following parts by weight:Flos Trollii
10 parts, 3 parts of Caulis et Folium Chrysanthemi segeti, 3 parts of sweet potato leaves and stemses superfine powder described in embodiment 1,1 part of Radix Glycyrrhizae, 1 part of xylitol and mixed accessories 18
Part, wherein, described mixed accessories are pressed by dextrin, the PVP alcoholic solution of 0.5% (W/W) and the corn cob superfine powder described in embodiment 3
1:0.5:0.05 weight is than composition.
Preparation method reference implementation example 5.
Embodiment 7, a kind of trollius chinensis granular agent
Described in the embodiment of the present invention 7, trollius chinensis granular agent is prepared from by the preparing raw material of following parts by weight:Flos Trollii
20 parts, 8 parts of Caulis et Folium Chrysanthemi segeti, 5 parts of sweet potato leaves and stemses superfine powder described in embodiment 1,10 parts of Radix Glycyrrhizae, 3 parts of xylitol and mixed accessories 45
Part, wherein, described mixed accessories press 1 by dextrin, the PVP alcoholic solution of 3% (W/W) and the corn cob superfine powder described in embodiment 4:
0.8:0.1 weight is than composition.
Preparation method reference implementation example 5.
Comparative example 1, a kind of trollius chinensis granular agent
Comparative example 1 is with the difference of embodiment 5:Remove Radix Glycyrrhizae, the parts by weight of Rhizoma Dioscoreae esculentae superfine powder increase to 9 parts, its
Remaining parameter and operation such as embodiment 5.
Comparative example 2, a kind of trollius chinensis granular agent
Comparative example 2 is with the difference of embodiment 5:Described mixed accessories are dextrin, and remaining parameter and operation are as embodiment
5.
Comparative example 3, a kind of trollius chinensis granular agent
Comparative example 3 is with the difference of embodiment 5:Described mixed accessories are pressed by the PVP alcoholic solution of dextrin and 2% (W/W)
1:0.6 weight ratio composition, remaining parameter and operation such as embodiment 5.
A kind of trollius chinensis granular agent of comparative example 4
Comparative example 4 is with the difference of embodiment 5:Described mixed accessories are by dextrin, the PVP alcoholic solution of 2% (W/W) and jade
Rice core superfine powder presses 1:1:1 weight is than composition.
Comparative example 5, a kind of trollius chinensis granular agent
Preparation method as described in identical step repeats embodiment 5, but step S3) in remove concentration filtrate I step,
Remaining parameter and operation such as embodiment 5.
Test example one, safety testing
Distinguish the granule that Example 5~7 and comparative example 1~5 are obtained, carry out acute toxicity test, feed within 30 days
Test and feeding test for 90 days.Result:The growing state of nutrition purposes, especially for feeding animals is good, and hematology and physico-chemical examination are normal.Therefore, this
Bright offer trollius chinensis granular agent has edible safety, suitable long-term drink.
Test example two, quality evaluation
Take the embodiment of the present invention 5~7 and granule described in comparative example 1~5, according to《Chinese Pharmacopoeia》2010 editions one attached
Record the character to each group granule, granularity, moisture, whole dissolution time, microbial limit, loss on drying and effect of pelletizing
Fruit is evaluated, and evaluation result is as shown in table 1.
Table 1 evaluation result
Note:【Character】:Brown yellow granule, uniformly, color and luster is unanimously qualified to granule;【Granularity】:Survey according to granulometry
Determine it is impossible to not can exceed that 15% by a sieve with No. five summations sieved can be passed through;【Moisture】:Survey according to aquametry
Fixed, take test sample about 1g, put 75 DEG C of drying under reduced pressure 5 hours, cool down 30 minutes, accurately weighed, then it is little to be dried 1 in said temperature
When, cooling, weigh, being less than 5mg to the double difference weighed, water content is qualified not less than 6%;【Dissolve
Property】:Take 1 bag of test sample, heating water 200ml, stir 5min, observe immediately, all dissolve, no muddy is qualified;【Microorganism limits
Degree】:According to microbial limit test inspection;【Loss on drying】In 80 DEG C of drying under reduced pressure to constant weight, less loss weight is less than 2%
For qualified.
From upper table 1:
Granule described in the embodiment of the present invention 5~7 has granule uniformly, the consistent feature of color and luster, and it pelletizes easily, molten
Going out property is excellent.
Compared with granule described in embodiment 5, described in comparative example 1~5, granule each side index has all declined.
It is to be noted that:Can be seen that from comparative example 2 result, be individually added into dextrin, be difficult to pelletize, difficult molding, and gained
The stripping property of granule is poor it is impossible to being sieved and can be passed through No. five summations sieved by No. one is each group highest, reaches 19.8%;Contrast
Example 3 adds PVP alcoholic solution on the basis of comparative example 2, and compared with comparative example 2, granulating efficiency has and substantially carries the granule of its gained
Rise, but the no significant change of the stripping property of granule and granularity;Comparative example 4 changes dextrin in mixed accessories, PVP alcoholic solution and Semen Maydiss
The proportioning of core superfine powder, the granule of its gained has declined compared with Example 5, but will than granule described in comparative example 2~3
Good.
Test example two, stability test
2.1 long-term room-temperature keep sample test
Example 5~7 and comparative example 2~4 commercial samples, under room temperature condition, kept sample test for a long time.Respectively at
3rd, 6,12 and 18 the end of month samplings, investigate its appearance character, melting, moisture and microbial limit, the results are shown in Table 2 institutes
Show.
Table 2 long-term room-temperature keeps sample result of the test
From upper table 2, the embodiment of the present invention 5~7 keeps sample after test through long-term room-temperature, the face shaping of sample, dissolves
Property, moisture and microbial limit have no significant change, and are valid up to a year and a half, have excellent stability.
It is to be noted that:Compared with sample described in embodiment 5, sample described in comparative example 2~4 keeps sample examination through long-term room-temperature
After testing, sample all has different degrees of change.Wherein, sample hygroscopicity described in comparative example 2,3 is stronger, and it is respectively at 6th month
Just there is with 12nd month moisture absorption phenomenon to occur, had at 12nd month and 18th month caking, mildew phenomena to occur, two groups of samples
Less stable, is unfavorable for preserving for a long time.
Test example three, clinical observation on the therapeutic effect
1. physical data
Select to have and invaded by cold-evil or the inappetence causing such as damp and hot, the volunteer of the weak symptom of heavy sensation of the body 250, the age
Between 18~35 years old, 250 volunteers are randomly divided into 5 groups, every group of 50 people, be respectively 5~7 groups of embodiment, 1 group of comparative example with
And 5 groups of comparative example.
2nd, Therapeutic Method
5 groups of embodiment:Trollius chinensis granular agent described in the embodiment of the present invention 5 (10g/ bag), 2 times a day, takes 1 pouch to use every time
Warm water is taken after mixing it with water, and 7 days is 1 course for the treatment of, continuously takes 2 courses for the treatment of;
6 groups of embodiment:Trollius chinensis granular agent described in the embodiment of the present invention 6 (10g/ bag), 2 times a day, takes 1 pouch to use every time
Warm water is taken after mixing it with water, and 7 days is 1 course for the treatment of, takes 1 course for the treatment of;
7 groups of embodiment:Trollius chinensis granular agent described in the embodiment of the present invention 7 (10g/ bag), 2 times a day, takes 1 pouch to use every time
Warm water is taken after mixing it with water, and 7 days is 1 course for the treatment of, takes 1 course for the treatment of;
1 group of comparative example:Trollius chinensis granular agent (10g/ bag) described in comparative example 1 of the present invention, 2 times a day, takes 1 pouch to use every time
Warm water is taken after mixing it with water, and 7 days is 1 course for the treatment of, takes 1 course for the treatment of;
5 groups of comparative example:Trollius chinensis granular agent (10g/ bag) described in comparative example 5 of the present invention, 2 times a day, takes 1 pouch to use every time
Warm water is taken after mixing it with water, and 7 days is 1 course for the treatment of, takes 1 course for the treatment of.
3rd, observation of curative effect.
3.1 curative effect index
(1) effective:Medication was taken food after 1~3 day substantially to be increased, the heavy sensation of the body weak phenomenon person of being wholly absent;
(2) effective:After taking medicine 3~7 days, symptom has been improved, and feed takes a turn for the better, the obvious alleviator of the weak phenomenon of heavy sensation of the body;
(3) invalid:The symptom person of being not improved after taking medicine 7 days.
3.2 statistical analysis application SPSS13.0 softwares carry out statistical procedures, and data to represent, examined with x2 by enumeration data
Test, measurement data is checked with t.
3.3 efficacy result
Table 3 efficacy result
Group | Number of cases | Effective (obvious effective rate %) | Effectively (effective percentage %) | Invalid (inefficiency %) | Total effective rate (%) |
5 groups of embodiment | 50 | 43 (86%) | 7 (14%) | 0 | 100 |
6 groups of embodiment | 50 | 40 (80%) | 10 (20%) | 0 | 100 |
7 groups of embodiment | 50 | 38 (76%) | 12 (24%) | 0 | 100 |
1 group of comparative example | 50 | 25 (50%) | 16 (32%) | 9 (18%) | 82 |
5 groups of comparative example | 50 | 20 (40%) | 18 (36%) | 12 (24%) | 76 |
From upper table 3, Granules in Treating described in the embodiment of the present invention 5~7 is invaded by cold-evil or the food causing such as damp and hot
It is intended to depressed, the weak symptom of heavy sensation of the body has significant effect, its total effective rate is up to 100%, significantly larger than comparative example 1 and comparative example
The therapeutic effect of granule described in 5 groups.
Claims (10)
1. a kind of trollius chinensis granular agent is it is characterised in that include the preparing raw material of following parts by weight:10~20 parts of Flos Trollii,
3~8 parts of Caulis et Folium Chrysanthemi segeti, 3~5 parts of sweet potato leaves and stemses superfine powder, 1~10 part of Radix Glycyrrhizae, 1~3 part of xylitol and 18~45 parts of mixed accessories,
Wherein, described mixed accessories press 1 by dextrin, the PVP alcoholic solution of 0.5~3% (W/W) and corn cob superfine powder:(0.5~0.8):
The weight of (0.05~0.1) is than composition.
2. trollius chinensis granular agent as claimed in claim 1 is it is characterised in that include the preparing raw material of following parts by weight:Gold
15 parts of Flos Nelumbinis, 6 parts of Caulis et Folium Chrysanthemi segeti, 4 parts of sweet potato leaves and stemses superfine powder, 5 parts of Radix Glycyrrhizae, 2 parts of xylitol and 26 parts of mixed accessories, wherein, institute
State mixed accessories by dextrin, the PVP alcoholic solution of 2% (W/W) and corn cob superfine powder by 1:0.6:0.06 weight is than composition.
3. trollius chinensis granular agent as claimed in claim 1 or 2 is it is characterised in that described sweet potato leaves and stemses superfine powder is by following step
Suddenly it is obtained:
Take fresh sweet potato stem and leaf, decontamination, clean, dry, be dried, after precomminution to 30~50 mesh, be broken into grain through super micron mill
Footpath is 20~50 μm of powder body, obtains final product.
4. trollius chinensis granular agent as claimed in claim 1 or 2 is it is characterised in that described corn cob superfine powder is by following steps
It is obtained:
Take the corn cob after drying, chopping, being broken into particle diameter through super micron mill after precomminution to 30~50 mesh is 32~45 μm
Powder body, obtains final product.
5. trollius chinensis granular agent as claimed in claim 1 or 2 is it is characterised in that described granule also includes lauryl alcohol sulphuric acid
0.1~0.3 part of magnesium.
6. a kind of method preparing described trollius chinensis granular agent as arbitrary in Claims 1 to 4 is it is characterised in that include following
Step:
A) the preparation of raw material fine powder:The preparation of described raw material fine powder includes tetra- steps of S1~S4:
S1, depletion Flos Nelumbinis, Caulis et Folium Chrysanthemi segeti and Radix Glycyrrhizae, clean, dry, and are ground into 60~70 mesh, add the distilled water of medical material 3~6 times amount
Decoct 1~3 time, filter, merge decoction liquor, relative density is 1.05~1.10 at 80~90 DEG C by decoction liquor evaporation and concentration
Concentrated solution I, cooling, standby;
S2, be slowly added dropwise while stirring toward in above-mentioned concentrated solution I described concentrated solution I 1~2 times amount 50~60% ethanol solution
Carry out a precipitate with ethanol, after standing overnight, take supernatant, precipitate is washed with 50~60% ethanol solution, cleaning mixture and supernatant
Merge to obtain filtrate I, decompression recycling ethanol;
S3, by filtrate I again evaporation and concentration relative density at 80~90 DEG C be 1.15~1.25 concentrated solution II, add concentrate
The ethanol solution of the 80~90% of liquid II 2~3 times amount carries out secondary precipitate with ethanol, takes supernatant after standing overnight, precipitate with 80~
90% ethanol solution washing, cleaning mixture merges to obtain filtrate II, decompression recycling ethanol with supernatant;
S4, filtrate II is concentrated into the thick paste that relative density at 80~90 DEG C is 1.30~1.35, by above-mentioned thick paste through spray dried
Dry one-tenth extract powder, adds sweet potato leaves and stemses superfine powder, mix homogeneously, obtains raw material fine powder;
B) toward in above-mentioned raw material fine powder, add xylitol and mixed accessories, mix, be pressed into thick piece in advance, pulverize, sieve, obtain final product.
7. the method for trollius chinensis granular agent as claimed in claim 6 is it is characterised in that described step A) described in sweet potato leaves and stemses
Superfine powder is obtained by following steps:
Take fresh sweet potato stem and leaf, decontamination, clean, dry, be dried, after precomminution to 30~50 mesh, be broken into grain through super micron mill
Footpath is 20~50 μm of powder body, obtains final product.
8. the method for trollius chinensis granular agent as claimed in claim 6 is it is characterised in that described step B) described in mixed accessories
Press 1 by dextrin, the PVP alcoholic solution of 0.5~3% (W/W) and corn cob superfine powder:(0.5~0.8):The weight of (0.05~0.1)
Than composition.
9. the method for trollius chinensis granular agent as claimed in claim 8 is it is characterised in that described step B) described in mixed accessories
Press 1 by dextrin, the PVP alcoholic solution of 0.5~3% (W/W) and corn cob superfine powder:0.6:0.06 weight is than composition.
10. the method for trollius chinensis granular agent as claimed in claim 6 is it is characterised in that described step B) also include toward described
0.1~0.3 part of magnesium laurylsulfate is added in raw material fine powder.
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WO2018099493A1 (en) * | 2016-11-29 | 2018-06-07 | 广东大鹏医药科技有限公司 | Tropaeolum majus granules and preparation method therefor |
CN109541085A (en) * | 2018-10-11 | 2019-03-29 | 河北中医学院 | The preparation method and detection method of a kind of pale purple Flos Trollii extract and its instant solid particle |
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CN1522581A (en) * | 2003-02-18 | 2004-08-25 | 戚海燕 | Edible and skin-care milk powder |
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CN103082277A (en) * | 2011-10-28 | 2013-05-08 | 江苏徐州甘薯研究中心 | Medicinal sweet potato Simon I leaf concentrated oral liquid and preparation method thereof |
CN103125661A (en) * | 2011-11-23 | 2013-06-05 | 汤汉忠 | Manufacturing method of heat-clearing internal heat-relieving tea |
CN103432186B (en) * | 2013-08-30 | 2015-08-12 | 遂成药业股份有限公司 | A kind of preparation method of Herba seu Flos Convolvuli arvensis granule |
CN105230884A (en) * | 2015-10-29 | 2016-01-13 | 长沙奥佳信息科技有限公司 | Preparation method of substituting tea for treating chronic pharyngitis |
CN106389966B (en) * | 2016-11-25 | 2019-06-18 | 广东大鹏医药科技有限公司 | A kind of Chinese globeflower buccal tablets and preparation method thereof |
CN106389776B (en) * | 2016-11-29 | 2019-04-05 | 广东大鹏医药科技有限公司 | A kind of trollius chinensis granular agent and preparation method thereof |
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CN102188506A (en) * | 2011-05-12 | 2011-09-21 | 承德天原药业有限公司 | Trollius chinensis granule preparation and preparation method thereof |
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CN109541085A (en) * | 2018-10-11 | 2019-03-29 | 河北中医学院 | The preparation method and detection method of a kind of pale purple Flos Trollii extract and its instant solid particle |
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