CN106075125A - A kind of YIXUANNING JIAONANG and preparation method thereof - Google Patents
A kind of YIXUANNING JIAONANG and preparation method thereof Download PDFInfo
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- CN106075125A CN106075125A CN201610542432.4A CN201610542432A CN106075125A CN 106075125 A CN106075125 A CN 106075125A CN 201610542432 A CN201610542432 A CN 201610542432A CN 106075125 A CN106075125 A CN 106075125A
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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)
- A61K36/899—Poaceae or Gramineae (Grass family), e.g. bamboo, corn or sugar cane
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/24—Heavy metals; Compounds thereof
- A61K33/26—Iron; Compounds thereof
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K35/00—Medicinal preparations containing materials or reaction products thereof with undetermined constitution
- A61K35/56—Materials from animals other than mammals
- A61K35/618—Molluscs, e.g. fresh-water molluscs, oysters, clams, squids, octopus, cuttlefish, snails or slugs
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/06—Fungi, e.g. yeasts
- A61K36/07—Basidiomycota, e.g. Cryptococcus
- A61K36/076—Poria
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- 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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- 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
- A61K36/287—Chrysanthemum, e.g. daisy
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- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/53—Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
- A61K36/539—Scutellaria (skullcap)
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- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/65—Paeoniaceae (Peony family), e.g. Chinese peony
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- 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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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/73—Rosaceae (Rose family), e.g. strawberry, chokeberry, blackberry, pear or firethorn
- A61K36/734—Crataegus (hawthorn)
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- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/75—Rutaceae (Rue family)
- A61K36/752—Citrus, e.g. lime, orange or lemon
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- 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)
- A61K36/81—Solanaceae (Potato family), e.g. tobacco, nightshade, tomato, belladonna, capsicum or jimsonweed
- A61K36/815—Lycium (desert-thorn)
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- 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)
- A61K36/888—Araceae (Arum family), e.g. caladium, calla lily or skunk cabbage
- A61K36/8884—Arisaema, e.g. Jack in the pulpit
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- 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
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- 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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- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- 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 present invention provides the preparation method of a kind of YIXUANNING JIAONANG, take Fructus Xanthii (parched) 20g, Flos Chrysanthemi 15g, Arisaema Cum Bile 15g, Radix Scutellariae 15g, Caulis Bambusae In Taenia 15g, Concha Ostreae (calcined) 20g, Fructus Crataegi 10g, Pericarpium Citri Reticulatae 15g, Radix Paeoniae Alba 15g, the pig iron fall 15g, Poria 20g, Fructus Lycii 20g, above 12 tastes, add the water of 10 times of weight of medical material, and use distinctive concentration and drying equipment, in the YIXUANNING JIAONANG prepared, Determination of Total Glucosides of Paeony is high, the application in the concurrent suppression African green monkey kidney Vero E6 cell proliferation of preparation now.
Description
Technical field
The present invention relates to technical field of extraction of Chinese traditional medicine, be specifically related to a kind of YIXUANNING JIAONANG and preparation method thereof.
Background technology
YIXUANNING JIAONANG energy suppressing the hyperactive liver and subsiding YANG, pathogenic fire reducing clearing away phlegm, spleen invigorating of nourishing blood, expelling wind and clearing away heat, cure mainly excessive rising of liver-YANG, QI and blood deficiency
Type vertigo.Preparation method of the prior art, technique is coarse, backward, and impurity is many, and active constituent content is low, causes patient to use
Measure excessive, it has not been convenient to take, had a strong impact on this product and applied clinically.
Summary of the invention
Goal of the invention: in order to solve the problems referred to above, it is an object of the invention to provide a kind of YIXUANNING JIAONANG and preparation thereof
Method.
Technical scheme: it is an object of the invention to by following scheme realization:
A kind of YIXUANNING JIAONANG, preparation method is: take Fructus Xanthii (parched) 20g, Flos Chrysanthemi 15g, Arisaema Cum Bile 15g, Radix Scutellariae 15g, bamboo
Eat 15g, Concha Ostreae (calcined) 20g, Fructus Crataegi 10g, Pericarpium Citri Reticulatae 15g, Radix Paeoniae Alba 15g, the pig iron fall 15g, Poria 20g, Fructus Lycii 20g, and above 12
Taste, adds the water of 10 times of weight of medical material, soaks 0.5h, decocts 1 hour, filters, and medicinal residues add the water of 8 times of weight of medical material, decocts 1
Hour, medicinal liquid leaches, and merges twice decoction liquor, and being concentrated into 60 DEG C of relative densities is 1.05, adds ethanol and makes the volume hundred of alcohol content
Proportion by subtraction reaches 75%, stirs, and stands, and filters, and when filtrate is concentrated into 65 DEG C, relative density is 1.25, and reclaims ethanol, obtains concentrated solution,
Use supercritical extraction, obtain supercritical extract, continue to concentrate, concentrated solution is dried, pelletize, encapsulating capsule, obtain YIXUANNING
Capsule.
Described YIXUANNING JIAONANG, in above-mentioned preparation method, supercritical extraction method is: joined by water extract-alcohol precipitation concentrated solution
In CO2 supercritical extraction device, ethanol is as entrainer, and it is 4-6% that entrainer accounts for the percent by volume of total extractant, extraction pressure
Power 15-30MPa, temperature 30-50 DEG C, CO2 flow 1-3ml/g crude drug min, extraction time 150-180min, obtain supercritical extraction
Taking thing, optimum condition is: the percent by volume that described CO2 supercritical extraction entrainer accounts for total extractant is 5%, described CO2
Extracting pressure 20MPa of supercritical extraction, temperature 40 DEG C, CO2 flow 2ml/g crude drug min, extraction time 160min.
Described YIXUANNING JIAONANG, concentrates for three times in above-mentioned preparation method and uses device, including tank body, be arranged on described tank body
On charging aperture and be arranged on the discharge nozzle of described tank base, described discharge nozzle is provided with discharge valve and filter,
It is provided with shaft in described tank body, described shaft is provided with stirring paddle, be provided with and described stirring at the top of described tank body
The stirring motor that axle is connected, the diapire in described tank body is provided with vibrations chamber, is provided with jolting plate at described vibrations intracavity, in institute
State and be provided with electromagnetic shaker between jolting plate and described vibrations chamber, the sidewall in described tank body is provided with cavity, at described jolting plate
End face be provided with scraper plate, between described scraper plate and described cavity, be provided with telescopic cylinder, described scraper plate is at described telescopic cylinder
Effect is lower realizes the scraping to jolting plate surface, is provided with the discharging being connected with described discharge nozzle at the center of described jolting plate
Mouthful.
Described YIXUANNING JIAONANG, in above-mentioned preparation method, jolting plate described in enrichment facility sets with the junction in described vibrations chamber
There is sealing metal bar, described tank body is provided with the shake control device being connected with described electromagnetic shaker.
Described YIXUANNING JIAONANG, in above-mentioned preparation method, the bottom of scraper plate described in enrichment facility is provided with metal scraping layer, institute
State metal scraping layer to be pressed on described jolting plate, described tank body is provided with the extension and contraction control being connected with described telescopic cylinder
Button.
Described YIXUANNING JIAONANG, is provided with water tester in tank body described in enrichment facility in above-mentioned preparation method, described
Cooler it is provided with in discharge nozzle.
Described YIXUANNING JIAONANG, is dried in above-mentioned preparation method and uses device, including body, be arranged in described body
Axis, the rotation being arranged on described axis outer wall holds dish, is provided with vibration motor in the lower end of described axis, at described body
Top be provided with vapours conveyance conduit, it is characterised in that: in described axis, be provided with cavity, be provided with at the top of described axis
Disk, described disk is arranged on described rotation and holds the top of dish, is provided with the most penetrating pore, described on described disk
It is provided with the heat conduction mast being connected with described cavity in disk, in described cavity, is provided with electrical heating block, on described heat conduction mast
Being provided with heat conduction thorn post, described heat conduction thorn post stretches in described pore, is provided with temperature sensor, at described cavity in described body
Inside being provided with the driver being connected with described temperature sensor, described driver switchs with the control of described electrical heating block and is connected
Connect.
Described YIXUANNING JIAONANG, in above-mentioned preparation method, pore described in dry use device is the loudspeaker that big bottom, top is little
Shape hole, described heat conduction thorn post stretches into the middle part in described horn-like hole, is provided with the most penetrating conduction net on described horn-like hole
Hole.
Described YIXUANNING JIAONANG, is dried in above-mentioned preparation method and uses the bottom surface of body described in device to be provided with chamber door, described
Chamber door is arranged on to rotate and holds the lowermost end of dish, and described heat conduction mast be silver-colored or aluminum or copper mast.
The application in preparation suppression African green monkey kidney Vero-E6 cell proliferation of the described YIXUANNING JIAONANG.
In prior art, YIXUANNING JIAONANG uses the method that water puies forward, and technique is coarse, backward, and impurity is many, causes patient's consumption
Excessive, it has not been convenient to take, in YIXUANNING JIAONANG prepared by the present invention, Radix Paeoniae Alba total glucosides yield increases, and content is high, dense in the present invention
Contracting device structure is simple, simple operation, it is provided with jolting plate and electromagnetic shaker, and is additionally provided with scraper plate and is connected with described scraper plate
Telescopic cylinder, can effectively prevent tank base from luming, be greatly improved the efficiency of heating surface to a certain extent, efficiently solves tradition skill
Caking bottom easily occurring in art Chinese medicinal concentration equipment and affect the technical deficiency of the efficiency of heating surface, stability in use is good and the suitability
By force, the stable effective ingredients of medicine is not destroyed.This drying equipment structure is simple, and simple operation is provided with circle at the top of axis
Dish, and on disk, it is provided with pore, vapours can be made to pass through disk, and in axis, be provided with electrical heating block and heating column
Bar, can start electrical heating block as required, and realize temperature transfer by heat conduction mast, and enter with by the vapours of disk
Row mixing, thereby may be ensured that the temperature of vapours, and regulation performance is good, and stability in use is strong, efficiently solves in conventional art
The uncontrollable technical deficiency of temperature in vapours heating drier.And find that described YIXUANNING JIAONANG is green in preparation suppression Africa
Application in monkey kidney Vero-E6 cell proliferation.
Accompanying drawing explanation
In order to make present disclosure be more likely to be clearly understood, below according to specific embodiment and combine accompanying drawing, right
The present invention is described in further detail, wherein:
Fig. 1 is the structural representation of enrichment facility of the present invention.
Fig. 2 is the structural representation of drying device of the present invention.
Detailed description of the invention
Form by the following examples, is described in further detail the foregoing of the present invention again, but should be by this
Being interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to Examples below, all technology realized based on foregoing of the present invention are equal
Belong to the scope of the present invention.
Embodiment 1
Take Fructus Xanthii (parched) 20g, Flos Chrysanthemi 15g, Arisaema Cum Bile 15g, Radix Scutellariae 15g, Caulis Bambusae In Taenia 15g, Concha Ostreae (calcined) 20g, Fructus Crataegi 10g, old
Skin 15g, Radix Paeoniae Alba 15g, the pig iron fall 15g, Poria 20g, Fructus Lycii 20g, and above 12 tastes add the water of 10 times of weight of medical material, soak
0.5h, decocts 1 hour, filters, and medicinal residues add the water of 8 times of weight of medical material, decoct 1 hour, and medicinal liquid leaches, and merges twice decoction
Liquid, being concentrated into 60 DEG C of relative densities is 1.05, adds ethanol and makes the percent by volume of alcohol content reach 75%, stirs, stand, filter,
When filtrate is concentrated into 65 DEG C, relative density is 1.25, and reclaims ethanol, obtains concentrated solution, uses supercritical extraction, obtains supercritical extraction
Take thing, continue to concentrate, concentrated solution is dried, pelletize, encapsulating capsule, obtain YIXUANNING JIAONANG.
The preparation method of described YIXUANNING JIAONANG, described supercritical extraction method is: joined by water extract-alcohol precipitation concentrated solution
In CO2 supercritical extraction device, ethanol is as entrainer, and it is 4% that entrainer accounts for the percent by volume of total extractant, extracting pressure
30MPa, temperature 30 DEG C, CO2 flow 3m1/g crude drug min, extraction time 150min, obtain supercritical extract.
See Fig. 1: the preparation method of described YIXUANNING JIAONANG, above-mentioned No. three enrichment facilities, including tank body 1, be arranged on described
Charging aperture on tank body 12 and be arranged on the discharge nozzle 3 bottom described tank body 1, is provided with discharge valve 4 He on described discharge nozzle 3
Filter 5, is provided with shaft 6 in described tank body 1, is provided with stirring paddle 7 on described shaft 6, at the top of described tank body 1
Being provided with the stirring motor 8 being connected with described shaft 6, the diapire in described tank body 1 is provided with vibrations chamber 9, in described vibrations
It is provided with jolting plate 10 in chamber 9, between described jolting plate 10 and described vibrations chamber 9, is provided with electromagnetic shaker 11, permissible by electromagnetic shaker
Make jolting plate shake, thus can effectively prevent drug particles from concentrating on jolting plate, thus drug particles can be prevented at jolting plate
Upper caking, the sidewall in described tank body 1 is provided with cavity 12, and the end face at described jolting plate 10 is provided with scraper plate 13, described
It is provided with telescopic cylinder 14 between scraper plate 13 and described cavity 12, telescopic cylinder can be controlled as required, make scraper plate at jolting plate
Surface scrape, thus part is concentrated at the drug particles on jolting plate surface and scrapes, described scraper plate 13 is at described telescopic cylinder
The effect of 14 is lower realizes the scraping to jolting plate 10 surface, is provided with at the center of described jolting plate 10 and is connected with described discharge nozzle 3
Logical discharging opening 15.
It is provided with sealing metal bar 16 in the junction of described jolting plate 10 with described vibrations chamber 9, described tank body is provided with
The shake control device 17 being connected with described electromagnetic shaker.
Be provided with metal scraping layer 18 in the bottom of described scraper plate, described metal scraping layer is pressed on described jolting plate,
Described tank body is provided with the extension and contraction control button 19 being connected with described telescopic cylinder.
In described tank body, it is provided with water tester 21, in described discharge nozzle, is provided with cooler 20.
See Fig. 2, the preparation method of described YIXUANNING JIAONANG, above-mentioned dry use device, including body 1, be arranged on described
Axis 2 in body 1, the rotation being arranged on described axis 2 outer wall holds dish 3, is provided with vibrations electricity in the lower end of described axis 2
Machine 4, is provided with vapours conveyance conduit 5 at the top of described body 1, is provided with cavity 6 in described axis 2, at described axis 2
Top is provided with disk 7, and described disk 7 is arranged on described rotation and holds the top of dish 3, is provided with the most penetrating on described disk 7
Pore 8, vapours through disk, enters rotation and holds dish, be provided with and leading that described cavity 6 is connected in described disk 7
Plume bar 9, is provided with electrical heating block 10 in described cavity 6, and described heat conduction mast 9 is provided with heat conduction thorn post 11, and described heat conduction is stung
Post 11 stretches in described pore 8, can be greatly improved the temperature mixing between vapours and electrical heating block, improves temperature controlled
Efficiency, is provided with temperature sensor 12 in described body 1, is provided with is connected with described temperature sensor 12 in described cavity 6
Driver 13, the control of described driver 13 and described electrical heating block 10 switchs and is connected.Temperature sensor in the present embodiment
Being the most already present product with driver, it has only to be attached according to the corresponding description of product in use.
Described pore is the horn-like hole that big bottom, top is little, and described heat conduction thorn post stretches into the middle part in described horn-like hole,
Described horn-like hole is provided with the most penetrating conduction mesh 14.
Be provided with chamber door 15 in the bottom surface of described body, described chamber door is arranged on and rotates the lowermost end holding dish.
Described heat conduction mast is silver or aluminum or copper mast.
Embodiment 2
Take Fructus Xanthii (parched) 20g, Flos Chrysanthemi 15g, Arisaema Cum Bile 15g, Radix Scutellariae 15g, Caulis Bambusae In Taenia 15g, Concha Ostreae (calcined) 20g, Fructus Crataegi 10g, old
Skin 15g, Radix Paeoniae Alba 15g, the pig iron fall 15g, Poria 20g, Fructus Lycii 20g, and above 12 tastes add the water of 10 times of weight of medical material, soak
0.5h, decocts 1 hour, filters, and medicinal residues add the water of 8 times of weight of medical material, decoct 1 hour, and medicinal liquid leaches, and merges twice decoction
Liquid, being concentrated into 60 DEG C of relative densities is 1.05, adds ethanol and makes the percent by volume of alcohol content reach 75%, stirs, stand, filter,
When filtrate is concentrated into 65 DEG C, relative density is 1.25, and reclaims ethanol, obtains concentrated solution, uses supercritical extraction, obtains supercritical extraction
Take thing, continue to concentrate, concentrated solution is dried, pelletize, encapsulating capsule, obtain YIXUANNING JIAONANG.
The preparation method of described YIXUANNING JIAONANG, described supercritical extraction method is: joined by water extract-alcohol precipitation concentrated solution
In CO2 supercritical extraction device, ethanol is as entrainer, and it is 6% that entrainer accounts for the percent by volume of total extractant, extracting pressure
15MPa, temperature 50 C, CO2 flow 1m1/g crude drug min, extraction time 180min, obtain supercritical extract.
Concentrate with drying device ibid.
Embodiment 3
Take Fructus Xanthii (parched) 20g, Flos Chrysanthemi 15g, Arisaema Cum Bile 15g, Radix Scutellariae 15g, Caulis Bambusae In Taenia 15g, Concha Ostreae (calcined) 20g, Fructus Crataegi 10g, old
Skin 15g, Radix Paeoniae Alba 15g, the pig iron fall 15g, Poria 20g, Fructus Lycii 20g, and above 12 tastes add the water of 10 times of weight of medical material, soak
0.5h, decocts 1 hour, filters, and medicinal residues add the water of 8 times of weight of medical material, decoct 1 hour, and medicinal liquid leaches, and merges twice decoction
Liquid, being concentrated into 60 DEG C of relative densities is 1.05, adds ethanol and makes the percent by volume of alcohol content reach 75%, stirs, stand, filter,
When filtrate is concentrated into 65 DEG C, relative density is 1.25, and reclaims ethanol, obtains concentrated solution, uses supercritical extraction, obtains supercritical extraction
Take thing, continue to concentrate, concentrated solution is dried, pelletize, encapsulating capsule, obtain YIXUANNING JIAONANG.
The preparation method of described YIXUANNING JIAONANG, described supercritical extraction method is: joined by water extract-alcohol precipitation concentrated solution
In CO2 supercritical extraction device, ethanol is as entrainer, and it is 5% that entrainer accounts for the percent by volume of total extractant, described CO2
Extracting pressure 20MPa of supercritical extraction, temperature 40 DEG C, CO2 flow 2ml/g crude drug min, extraction time 160min, obtain super
Critical extract.
Concentrate with drying device ibid.
Above-described embodiment Chinese medicine all meets standards of pharmacopoeia.
Embodiment 4: Determination of Total Glucosides of Paeony determination experiment research data in YIXUANNING JIAONANG of the present invention
1.1 Experimental agents: YIXUANNING JIAONANG of the present invention: prepare by embodiment 1-3 method.Matched group uses ministry standard,
Common method for concentration prepares YIXUANNING JIAONANG.
1.2 instruments: high performance liquid chromatograph system includes high performance liquid chromatograph (Waters 515);P200 high-pressure pump;
Waters 2487 UV-detector and GJ605 type high pressure six-way injection valve;Data acquisition and process use the work of HS chromatographic data
Stand V4.0+ (Hangzhou English spectrum science and technology)
1.3 condition determinations: use high performance liquid chromatography, with octadecylsilane chemically bonded silica for fixing phase, acetonitrile-
0.1% phosphoric acid (25:75) is flowing phase, detects wavelength 230nm, flow velocity 1.0mL/min, measures benzoic acid content, thus calculate
Go out Determination of Total Glucosides of Paeony.
1.4 experimental result
Determination of Total Glucosides of Paeony measurement result in YIXUANNING JIAONANG prepared by each embodiment
Sample source | Determination of Total Glucosides of Paeony (%) |
Embodiment 1 | 1.46 |
Embodiment 2 | 1.68 |
Embodiment 3 | 1.73 |
Matched group | 0.53 |
According to the result of the test of upper table, in YIXUANNING JIAONANG prepared by embodiment of the present invention 1-3, peaceful Radix Paeoniae Alba total glucosides contains
Amount is apparently higher than matched group.
Embodiment 5: the experimentation data of YIXUANNING JIAONANG of the present invention suppression African green monkey kidney Vero-E6 cell proliferation
1 experiment material
1.1 experiment cell strains
African green monkey kidney Vero-E6 cell, Jilin Province just with Pharmaceutical Group Plc laboratory cell storehouse, DMEM
+ 10%FBS cellar culture.
1.2 Experimental agents
Drugs: YIXUANNING JIAONANG of the present invention: prepare by embodiment 1 method.
Medicinal liquid liquid storage: weigh 100mg YIXUANNING JIAONANG, is dissolved in 5ml dehydrated alcohol, and 0.2 μm filter filters, 500 μ l
Doff pipe subpackage ,-20 DEG C of storages, 0.2 μm filter filters dehydrated alcohol in case matched group is used simultaneously.
1.3 experiment reagent
DMEM (GIBCO company Cat.No.12100-061Lot.No.758137);Hyclone (Hangzhoupro, sky, Zhejiang biology section
Skill company limited Lot.No.100419);NaHCO3 (the long hundred million chemical reagent company limited Cat.No.11810-in Shanghai
033Lot.No.1088387);Trypsin (AMRESCO company lot number: 2010/04);EDTA (AMRESCO company lot number:
2009/10);Penicillin G Sodium Salt (AMRESCO company lot number: 2010242);Streptomycin
Sulfate (AMRESCO company lot number: 2010382);Dehydrated alcohol (Nanjing Chemistry Reagent Co., Ltd.'s lot number:
080310182);MTT (Biosharp lot number: 0793);PBS (laboratory autogamy);1.4 experiment equipment
Lycra inverted microscope (Germany Leica model: DM1L);Visible-ultraviolet light microwell plate detector (MD company of the U.S.
Model: SPECTRA MAX 190);CO2 incubator (FORMA model: 3111);Super-clean bench (safe and sound company of Su Jing group manufacture type
Number: SW-CJ-ZFD);Pure water instrument (Spring company of U.S. model: S/N 020579);Accurate pipettor (Gilson Inc of France
Model: P2);Electronic balance (Sai Duolisi company limited of Germany model: BT323S);Full-automatic high-pressure autoclave (Japan SANYO
Company's model: MLS-3020);Table electrothermal air dry oven (Shanghai precision experimental facilities company model: DHG9123A);Refrigerator
(Siemens Company's model: KG18V21TI);Liquid nitrogen container (CBS model: 2001);Low speed centrifuge (Anting Scientific Instrument Factory, Shanghai
Model: KA-1000);0.2 μm filter (MILLIPORE model: SLGP033RB);10cm culture dish (NEST company), 96 hole trainings
Support plate (NEST company);Cell counting count board;Centrifuge tube, pipet, Tips are some.
2 experimental techniques
1) African green monkey kidney Vero-E6 cell DMEM+10%FBS in 37 DEG C, 5%CO2 carry out cellar culture (10cm train
Support ware), when cell grows to logarithmic (log) phase, collect cell, discard culture fluid, PBS rinses 3 times, adds 3ml0.25% Trypsin
Enzyme-0.04%EDTA, after 37 DEG C of digestion 2min, is added thereto in 5ml complete medium and reacts, by its turn after piping and druming cell
Entering in centrifuge tube, 1000rpm is centrifuged 5min, adjusts 3 × 104/ml of concentration of cell suspension.
2) entering in 96 well culture plates by cell kind, every hole adds cell suspension 180 μ l, and culture plate is put in cell culture incubator
(37 DEG C, 5%CO2) cellar culture.
3) according to cell growth status, general long to 50%-70%, add YIXUANNING JIAONANG solution, continue to cultivate 24h.
4) add 20 μ l MTT solution (5mg/ml, i.e. 0.5%MTT) after 24h, continue to cultivate 4h.
5) after 4h, buckle method removes supernatant, pats dry gently with absorbent paper, and every hole adds 200 μ l dimethyl sulfoxide, puts shaking table
Upper low-speed oscillation 10min, makes crystal fully dissolve.The light absorption value in each hole is measured at enzyme-linked immunosorbent assay instrument 490nm.
6) arranging background (being not added with cell, only add culture fluid), (cell, the medicine dissolution of same concentrations are situated between control wells simultaneously
Matter, culture fluid, MTT, dimethyl sulfoxide), often group sets 6 multiple holes.
7) suppression ratio of cell is represented by result with medicine:
Cell proliferation suppression ratio (%)=(control wells OD value-dosing holes OD value)/control wells OD value × 100%.Experiment weight
Multiple 3 times.
3 statistical dispositions
Use the correlation analysis in Microsoft Excel 2003 software and Student t inspection, data with mean ±
S.D. represent.
4 experimental results
Statistical result showed after mtt assay experiment, compares with matched group, when dosage reaches 5mg/ml, to African green monkey kidney
Vero-E6 cell inhibitory effect variant (P < 0.05), dosage this difference when 10mg/ml has significance (P < 0.01), when
Dosage reaches there is pole significant difference (P < 0.001) during 15-20mg/ml.
YIXUANNING JIAONANG is to African green monkey kidney Vero-E6 cell inhibitory effect influence research
Note: compare with matched group, * P < 0.01;**P<0.001
5 experiment conclusion
YIXUANNING JIAONANG can suppress African green monkey kidney Vero-E6 cell proliferation, reduces African green monkey kidney Vero-E6 cell
Cell growing number, this effect is dose dependent.
Claims (10)
1. a YIXUANNING JIAONANG, it is characterised in that preparation method is: take Fructus Xanthii (parched) 20g, Flos Chrysanthemi 15g, Arisaema Cum Bile 15g, Huang
A kind of reed mentioned in ancient books 15g, Caulis Bambusae In Taenia 15g, Concha Ostreae (calcined) 20g, Fructus Crataegi 10g, Pericarpium Citri Reticulatae 15g, Radix Paeoniae Alba 15g, the pig iron fall 15g, Poria 20g, Fructus Lycii 20g,
Above 12 tastes, add the water of 10 times of weight of medical material, soak 0.5h, decoct 1 hour, filter, and medicinal residues add 8 times of weight of medical material
Water, decocts 1 hour, and medicinal liquid leaches, and merges twice decoction liquor, and being concentrated into 60 DEG C of relative densities is 1.05, adds ethanol and makes alcohol content
Percent by volume reach 75%, stirring, stand, filter, when filtrate is concentrated into 65 DEG C, relative density is 1.25, and reclaims ethanol,
Obtain concentrated solution, use supercritical extraction, obtain supercritical extract, continue to concentrate, concentrated solution is dried, pelletize, encapsulating capsule,
Obtain YIXUANNING JIAONANG.
YIXUANNING JIAONANG the most according to claim 1, it is characterised in that in described preparation method, supercritical extraction method is: will
Water extract-alcohol precipitation concentrated solution joins CO2In supercritical extraction device, ethanol is as entrainer, and entrainer accounts for the volume of total extractant
Percentage ratio is 4-6%, extracting pressure 15-30MPa, temperature 30-50 DEG C, CO2Flow 1-3m1/g crude drug min, extraction time
150-180min, obtains supercritical extract, and optimum condition is: described CO2Supercritical extraction entrainer accounts for the body of total extractant
Long-pending percentage ratio is 5%, described CO2Extracting pressure 20MPa of supercritical extraction, temperature 40 DEG C, CO2Flow 2ml/g crude drug min,
Extraction time 160min.
YIXUANNING JIAONANG the most according to claim 1, it is characterised in that concentrate for three times in described preparation method and use device, bag
Include tank body, the charging aperture being arranged on described tank body and the discharge nozzle being arranged on described tank base, described discharge nozzle sets
There are discharge valve and filter, in described tank body, are provided with shaft, described shaft is provided with stirring paddle, at described tank body
Top be provided with the stirring motor being connected with described shaft, the diapire in described tank body be provided with vibrations chamber, in described shake
Dynamic intracavity is provided with jolting plate, is provided with electromagnetic shaker, on the sidewall in described tank body between described jolting plate and described vibrations chamber
Being provided with cavity, the end face at described jolting plate is provided with scraper plate, is provided with telescopic cylinder between described scraper plate and described cavity, described
Scraper plate realizes the scraping to jolting plate surface under the effect of described telescopic cylinder, is provided with described at the center of described jolting plate
The discharging opening that discharge nozzle is connected.
YIXUANNING JIAONANG the most according to claim 3, it is characterised in that jolting plate described in enrichment facility in described preparation method
It is provided with sealing metal bar with the junction in described vibrations chamber, described tank body is provided with the vibrations control being connected with described electromagnetic shaker
Device processed.
YIXUANNING JIAONANG the most according to claim 3, it is characterised in that scraper plate described in enrichment facility in described preparation method
Bottom is provided with metal scraping layer, and described metal scraping layer is pressed on described jolting plate, is provided with and stretches with described on described tank body
The extension and contraction control button that contracting cylinders connects.
YIXUANNING JIAONANG the most according to claim 3, it is characterised in that in described preparation method in tank body described in enrichment facility
It is provided with water tester, in described discharge nozzle, is provided with cooler.
YIXUANNING JIAONANG the most according to claim 1, it is characterised in that be dried in described preparation method and use device, including machine
Body, is arranged on the axis in described body, and the rotation being arranged on described axis outer wall holds dish, sets in the lower end of described axis
There is vibration motor, be provided with vapours conveyance conduit at the top of described body, it is characterised in that: in described axis, it is provided with sky
Chamber, is provided with disk at the top of described axis, and described disk is arranged on described rotation and holds the top of dish, sets on described disk
There is the most penetrating pore, in described disk, be provided with the heat conduction mast being connected with described cavity, be provided with in described cavity
Electrical heating block, described heat conduction mast is provided with heat conduction thorn post, and described heat conduction thorn post stretches in described pore, sets in described body
Having temperature sensor, be provided with the driver being connected with described temperature sensor in described cavity, described driver is with described
The control switch of electrical heating block is connected.
YIXUANNING JIAONANG the most according to claim 7, it is characterised in that be dried described in use device thin in described preparation method
Hole is the horn-like hole that big bottom, top is little, and described heat conduction thorn post stretches into the middle part in described horn-like hole, in described horn-like hole
It is provided with the most penetrating conduction mesh.
YIXUANNING JIAONANG the most according to claim 7, it is characterised in that be dried in described preparation method and use machine described in device
The bottom surface of body is provided with chamber door, and described chamber door is arranged on and rotates the lowermost end holding dish, and described heat conduction mast is silver or aluminum or copper
Mast.
The most according to claim 1, YIXUANNING JIAONANG is in preparation suppression African green monkey kidney Vero-E6 cell proliferation
Application.
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102359941A (en) * | 2011-10-07 | 2012-02-22 | 通化正和药业有限公司 | Yixuanning capsule, its identification and content determining method |
CN103341074A (en) * | 2013-07-29 | 2013-10-09 | 通化茂祥制药有限公司 | Application of Yixuanning granules in preparation of medicaments for treating insomnia |
CN104840797A (en) * | 2015-05-28 | 2015-08-19 | 吉林省正和药业集团股份有限公司 | Preparation method and application of Yixuanning capsule |
-
2016
- 2016-07-11 CN CN201610542432.4A patent/CN106075125A/en not_active Withdrawn
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102359941A (en) * | 2011-10-07 | 2012-02-22 | 通化正和药业有限公司 | Yixuanning capsule, its identification and content determining method |
CN103341074A (en) * | 2013-07-29 | 2013-10-09 | 通化茂祥制药有限公司 | Application of Yixuanning granules in preparation of medicaments for treating insomnia |
CN104840797A (en) * | 2015-05-28 | 2015-08-19 | 吉林省正和药业集团股份有限公司 | Preparation method and application of Yixuanning capsule |
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Title |
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