CN110090251A - A kind of preparation method of Artemisia capillaris piece - Google Patents
A kind of preparation method of Artemisia capillaris piece Download PDFInfo
- Publication number
- CN110090251A CN110090251A CN201910474673.3A CN201910474673A CN110090251A CN 110090251 A CN110090251 A CN 110090251A CN 201910474673 A CN201910474673 A CN 201910474673A CN 110090251 A CN110090251 A CN 110090251A
- Authority
- CN
- China
- Prior art keywords
- water
- extract
- preparation
- dry
- ethyl alcohol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- A61K36/282—Artemisia, e.g. wormwood or sagebrush
-
- 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)
- A61K36/70—Polygonaceae (Buckwheat family), e.g. spineflower or dock
- A61K36/708—Rheum (rhubarb)
-
- 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)
- A61K36/74—Rubiaceae (Madder family)
- A61K36/744—Gardenia
-
- 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
- A61K9/2095—Tabletting processes; Dosage units made by direct compression of powders or specially processed granules, by eliminating solvents, by melt-extrusion, by injection molding, by 3D printing
-
- 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
- A61K9/28—Dragees; Coated pills or tablets, e.g. with film or compression coating
- A61K9/2806—Coating materials
- A61K9/2833—Organic macromolecular compounds
- A61K9/286—Polysaccharides, e.g. gums; Cyclodextrin
- A61K9/2866—Cellulose; Cellulose derivatives, e.g. hydroxypropyl methylcellulose
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
- A61P1/16—Drugs for disorders of the alimentary tract or the digestive system for liver or gallbladder disorders, e.g. hepatoprotective agents, cholagogues, litholytics
-
- 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
-
- 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
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
-
- 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
-
- 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
-
- 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
- A61K2236/55—Liquid-liquid separation; Phase separation
Landscapes
- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Public Health (AREA)
- Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Veterinary Medicine (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Epidemiology (AREA)
- Engineering & Computer Science (AREA)
- Microbiology (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Mycology (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Gastroenterology & Hepatology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
- Medicinal Preparation (AREA)
Abstract
The present invention relates to a kind of preparation method of Artemisia capillaris piece, this method comprises the steps of: (1) oriental wormwood is extracted with ethyl alcohol, macroporous resin purification, dry, obtains extract dry cream；(2) cape jasmine is extracted with water, macroporous resin purification, dry, obtains extract dry cream；(3) rheum officinale water extract-alcohol precipitation, supernatant concentration, ethyl acetate extraction concentration precipitate drying with alcohol precipitation, obtain Chinese rhubarb extract dry cream；(4) extract dried cream powder and auxiliary material mixing；(5) it pelletizes；(6) tabletting；(7) it is coated, the Artemisia capillaris piece of preparation is easy to carry, saves, and convenient to take, mobility of particle is good, and the finished product effective component rate of transform is high, and quality is stablized.
Description
Technical field
The present invention relates to a kind of preparation methods of Chinese materia medica preparation Artemisia capillaris piece.
Background technique
Cholestatic liver disease caused by a variety of causes belongs to the scope of Chinese medicine jaundice.It is burnt in retention of damp-heat in the interior, fumigate liver
Gallbladder, liver dysfunction, bile is excessive, is the Basic disease cause interpretation of the cause, onset and process of an illness.Sick position mainly in liver and gallbladder, taste, disease long also can and kidney.Common heat-clearing
The methods of dampness removing, activating microcirculation and removing stasis medicinal, cool blood, resolving sputum.
Common oral removing jaundice drug clinical at present mainly has Yin Zhi Huang effervescent tablet (oral solution), jaundice capillaris particle etc..Mattress
Cape jasmine Huang be capillary extract, capejasmine extract, scutelloside, Honegsukle flower P.E, jaundice capillaris particle be then by oriental wormwood, radix scutellariae,
Granule made of rheum officinale (system), Radix Glycyrrhizae, primary efficacy are clearing heat and promoting diuresis, removing jaundice subcutaneous ulcer.It is infected for treating acute and chronic icteric
Property hepatitis.The non-traditional classics side of the two, main function are clearing heat and detoxicating, lack dissolving stasis effect, do not embody traditional classical prescription and make
With feature, the raising of tcm clinical curative effect is limited.
For this disease, modern hospital also lacks effective therapeutic agent at present.Common s-adenosyl-L-methionine (the fourth two of clinic
Sulfonic acid Ademetionine) enteric coatel tablets and ursodesoxycholic acid etc., though the former can bilirubin reducing to a certain extent, it is total to chronic liver disease
It is unobvious and expensive that bilirubin slightly increases patient's effect.And the latter's main advantage is then embodied on drop GGT, AKP, drop
Bilirubin effect is limited.And above two drug is markedly less than in terms of mitigating patient suffering in the clinical symptoms for improving patient
Chinese medicine.
Yinchenhao Tang, Oriental Wormwood Decoction is the preferred prescription of clinical treatment yang jaundice, successive dynasties doctor first recorded in the treatise on Febrile Diseases of Han dynasty Zhang Zhongjing
Scholar has the greatest esteem it.Artemisia capillaris Tangyuan County side group becomes six liang of Artemisia capillaris, 14 pieces of cape jasmine, two liang of rheum officinale.Clinical and experiment
Promote bilirubin metabolism, anti-liver injury the study found that Yinchenhao Tang, Oriental Wormwood Decoction has, inhibit hepatocellular apoptosis, inhibit stellate cell activation
And the effect of collage synthesis.Seminar's early period confirms that Yinchenhao Tang, Oriental Wormwood Decoction has by three kinds of models such as bile duct ligation model, DMN models
There are apparent normalizing gallbladder to cure jaundice, alt-reducing and liver-protecting effect.But decoction is inconvenient to carry.
Summary of the invention
Goal of the invention: it is convenient to take for the ease of carrying, saving under the premise of ensuring curative effect, now provide a kind of mattress
The preparation method of old wormwood artemisia piece.
Technical solution:
A kind of preparation method of Artemisia capillaris piece, Artemisia capillaris piece are prepared by rheum officinale, oriental wormwood, Fructus Gardeniae extraction, the party
Method comprises the steps of: (1) rheum officinale water extract-alcohol precipitation, supernatant concentration, and ethyl acetate extraction concentration precipitates drying with alcohol precipitation,
Obtain Chinese rhubarb extract dry cream；(2) oriental wormwood is extracted with ethyl alcohol, macroporous resin purification, dry, obtains capillary extract dry cream；(3) cape jasmine
It is extracted with water, macroporous resin purification, it is dry, obtain capejasmine extract dry cream；(4) by be prepared three kinds of extract dry creams and auxiliary
Material mixing, granulation；(5) tabletting；(6) it is coated.
Above-mentioned preparation method, big yellow water described in step (1) extract 3 times, 1.5 hours every time, add 10 times of amount water for the first time,
Remaining adds 8 times of amount water twice, combined extract, and relative density when being concentrated into 60 DEG C is 1.10-1.15, lets cool to room temperature, adds 4
95% ethyl alcohol of amount again stands 24 hours, and precipitating is spare, and relative density when supernatant is concentrated into 60 DEG C is 1.10-1.15, with etc.
Volume of ethylacetate extracts 4 times, obtains gallic acid position after taking ethyl acetate layer to recycle ethyl acetate, mixes with alcohol precipitation precipitating dry
It is dry.
Above-mentioned preparation method, oriental wormwood described in step (2) are extracted 2 times with 75% ethyl alcohol, 1 hour every time, add 12 for the first time
Solvent is measured again and impregnates 2h, and second plus 8 times of amount solvents merge No. 2 extracting solutions, are concentrated under reduced pressure, and recycling ethyl alcohol adds to no alcohol taste
It is 0.1g crude drug/ml that water, which is diluted to density, and the filtering of 200 mesh gauzes stands, takes supernatant loading HPD200A macroporous resin column, on
Sample speed≤1BV/h, the complete water of loading rinse 1BV, elute 3BV with 50% ethyl alcohol with≤1BV/h speed, collect eluent, and 60 DEG C
Being concentrated under reduced pressure into density is 1.22-1.26g/ml, and 60 DEG C are dried under reduced pressure, and is crushed.
Above-mentioned preparation method, cape jasmine described in step (3) are extracted with water, and cape jasmine is ground into coarse powder, and water extracts 3 times, and every time 1
Hour, 14 times of amount water of first time simultaneously impregnate 2h, remaining adds 10 times of amount water twice, merges No. 3 extracting solutions, macroporous resin column loading
HPD200A macroreticular resin, diameter height ratio 1:7, loading speed≤3BV/h, loading is complete to be rinsed with water to colourless, with 5BV50% ethyl alcohol
It with≤3BV/h speed elution, is concentrated under reduced pressure, recycles ethyl alcohol, until density is 1.22-1.26g/ml, 60 DEG C are dried under reduced pressure, and are crushed.
Above-mentioned preparation method, 3 extract dry cream mixing, are added microcrystalline cellulose, polyvinyl pyrrole described in step (4)
Alkanone K30, low substituted hydroxy-propyl fiber, dry granulation, dry granulation technology use following technological parameter: process parameter control is such as
Under: grain made parameter is as follows: feeding motor: 4~12Hz；Tabletting motor: 12~22Hz；Crush motor: 5~15Hz；Whole grain motor:
12~22Hz.
Above-mentioned preparation method, step (6) coating, seed-coating machine parameter are as follows: temperature of charge: 40 DEG C~43 DEG C；Inlet air temperature:
70 DEG C~83 DEG C；Leaving air temp: 50 DEG C~80 DEG C；Rotation speed of fan: 800~1200rpm；Atomizing pressure: 1.5~3MPa.
Above-mentioned preparation method, Artemisia capillaris piece are prepared by following parts by weight medicinal material extract: 5~9 parts of rheum officinale, oriental wormwood 12~
15 parts, 3~9 parts of cape jasmine.
The utility model has the advantages that manufactured mobility of particle is good, the finished product effective component rate of transform is high, and quality is stablized.
Specific embodiment
Embodiment 1: 5 parts of rheum officinale, 15 parts of oriental wormwood, 3 parts of cape jasmine, preparation method are taken are as follows:
Big yellow water refluxing extraction 2 times, each 1h, 6 times of amount water, adds 1 times of amount, filtration, merging filtrate, concentration for the first time every time
It to density 1.10g/ml (60 DEG C), lets cool, is added the ethyl alcohol of 2 times of volumes, alcohol precipitation 12 hours.Alcohol hypostasis is spare, alcohol precipitation supernatant
Ethyl alcohol is recovered under reduced pressure to no alcohol taste (density is 1.15g/ml (60 DEG C)) in liquid, is extracted 2 times, is closed with the ethyl acetate of 1 times of volume
And ethyl acetate layer extract liquor, gallic acid position is obtained after recycling ethyl acetate, is uniformly mixed with alcohol hypostasis, (60 DEG C) is depressurized and does
It is dry, it crushes, obtains extract 1.
60% ethyl alcohol of oriental wormwood extracts 1 time, 1 hour every time, adds 10 times of amount solvents for the first time and impregnates 1h, and second plus 7 times
Solvent is measured, combined extract is concentrated under reduced pressure, recycling ethyl alcohol to no alcohol taste, and being diluted with water to density is 0.1g crude drug/ml, 200 mesh
Gauze filtering, stands, and takes supernatant loading HPD200A macroporous resin column, loading speed≤1BV/h, and the complete water of loading rinses 1BV,
With 40% ethyl alcohol with≤1BV/h speed elution 3BV, eluent is collected, it is 1.22g/ml that 60 DEG C, which are concentrated under reduced pressure into density, and 60 DEG C subtract
Pressure dry, pulverize, and obtain extract 2.
Cape jasmine is ground into coarse powder, and water extracts 2 times, and 1 hour every time, 12 times of amount water of first time, remaining added 8 times of amount water twice,
Merge No. 3 extracting solutions, macroporous resin column loading (HPD200A macroreticular resin, diameter height ratio 1:7), loading speed≤1BV/h, loading
It is complete to be rinsed with water to colourless, it is eluted with 3BV50% ethyl alcohol with≤1BV/h speed, is concentrated under reduced pressure, ethyl alcohol is recycled, until density is
1.22g/ml, 60 DEG C are dried under reduced pressure, and crush, obtain extract 3.
3 kinds of extracts are uniformly mixed, appropriate microcrystalline cellulose, 3% PVP K30,1% low substitution hydroxyl are added
Propyl cellulose is uniformly mixed, granulation.
After granulation, 1% magnesium stearate is added, three-dimensional mixer mixes, bladder type stamping, and slice weight 0.6g, every quite
In crude drug 3.8g.
It is coated using stomach dissolved film coating pre-mix dose, weight gain 1%.Seed-coating machine parameter is as follows:
Temperature of charge: 40 DEG C~43 DEG C
Inlet air temperature: 70 DEG C
Leaving air temp: 50 DEG C~80 DEG C
Rotation speed of fan: 800rpm.
Embodiment 2: 9 parts of rheum officinale, 12 parts of oriental wormwood, 9 parts of cape jasmine, preparation method are taken are as follows:
Big yellow water refluxing extraction 4 times, each 2h, 10 times of amount water, adds 2 times of amounts for the first time, filters, merging filtrate is dense every time
Density 1.15g/ml (60 DEG C) are reduced to, are let cool, are added the ethyl alcohol of 6 times of volumes, alcohol precipitation 36 hours.Alcohol hypostasis is spare, on alcohol precipitation
Ethyl alcohol is recovered under reduced pressure to no alcohol taste (density be 1.15g/ml (60 DEG C)) in clear liquid, is extracted 6 times with the ethyl acetate of 3 times of volumes,
Combined ethyl acetate layer extract liquor obtains gallic acid position after recycling ethyl acetate, is uniformly mixed with alcohol hypostasis, depressurize (60 DEG C)
It dry, pulverize, obtain extract 1.
90% ethyl alcohol of oriental wormwood extracts 3 times, 2 hours every time, adds 12 times of amount solvents for the first time and impregnates 2h, and second plus 9 times
Solvent is measured, combined extract is concentrated under reduced pressure, recycling ethyl alcohol to no alcohol taste, and being diluted with water to density is 0.3g crude drug/ml, 200 mesh
Gauze filtering, stands, and takes supernatant loading HPD200A macroporous resin column, loading speed≤3BV/h, and the complete water of loading rinses 3BV,
With 60% ethyl alcohol with≤3BV/h speed elution 5BV, eluent is collected, it is 1.26g/ml that 60 DEG C, which are concentrated under reduced pressure into density, and 60 DEG C subtract
Pressure dry, pulverize, and obtain extract 2.
Cape jasmine is ground into coarse powder, and water extracts 4 times, and 2 hours every time, 14 times of amount water of first time simultaneously impregnated 2h, remaining adds twice
12 times of amount water, merge No. 3 extracting solutions, macroporous resin column loading (HPD200A macroreticular resin, diameter height ratio 1:7), and loading speed≤
3BV/h, loading is complete to be rinsed with water to colourless, is eluted with 7BV70% ethyl alcohol with≤3BV/h speed, is concentrated under reduced pressure, recycles ethyl alcohol,
It is 1.26g/ml to density, 60 DEG C are dried under reduced pressure, and crush, obtain extract 3.
3 kinds of extracts are uniformly mixed, appropriate microcrystalline cellulose, 7% PVP K30,5% low substitution hydroxyl are added
Propyl cellulose is uniformly mixed, granulation.
Grain made parameter is as follows:
Feeding motor: 12Hz
Tabletting motor: 22Hz
Crush motor: 15Hz
Whole grain motor: 22Hz
After granulation, 1% magnesium stearate is added, three-dimensional mixer mixes, bladder type stamping, and slice weight 0.6g, every quite
In crude drug 3.8g.
It is coated using stomach dissolved film coating pre-mix dose, weight gain 1~3%.Seed-coating machine parameter is as follows:
Temperature of charge: 40 DEG C~43 DEG C
Inlet air temperature: 83 DEG C
Leaving air temp: 50 DEG C~80 DEG C
Rotation speed of fan: 1200rpm
Atomizing pressure: 3MPa.
Embodiment 3: 6 parts of rheum officinale, 12 parts of oriental wormwood, 6 parts of cape jasmine, preparation method are taken are as follows:
Big yellow water refluxing extraction 3 times, each 1.5h, 8 times of amount water, adds 2 times of amounts for the first time, filters, merging filtrate is dense every time
Density 1.15g/ml (60 DEG C) are reduced to, are let cool, are added the ethyl alcohol of 4 times of volumes, alcohol precipitation 24 hours.Alcohol hypostasis is spare, on alcohol precipitation
Ethyl alcohol is recovered under reduced pressure to no alcohol taste (density be 1.10g/ml (60 DEG C)) in clear liquid, is extracted 3 times with the ethyl acetate of equimultiple volume,
Combined ethyl acetate layer extract liquor obtains gallic acid position after recycling ethyl acetate, is uniformly mixed with alcohol hypostasis, depressurize (60 DEG C)
It dry, pulverize, obtain extract 1.
70% ethyl alcohol of oriental wormwood extracts 2 times, 1.5 hours every time, adds 11 times of amount solvents for the first time and impregnates 1.5h, add for the second time
8 times of amount solvents, combined extract are concentrated under reduced pressure, recycling ethyl alcohol to no alcohol taste, and being diluted with water to density is 0.2g crude drug/ml,
The filtering of 200 mesh gauzes, stands, and takes supernatant loading HPD200A macroporous resin column, loading speed≤2BV/h, and the complete water of loading rinses
2BV elutes 4BV with 45% ethyl alcohol with≤2BV/h speed, collects eluent, and it is 1.24g/ml that 60 DEG C, which are concentrated under reduced pressure into density, and 60
It DEG C is dried under reduced pressure, crushes, obtain extract 2.
Cape jasmine is ground into coarse powder, and water extracts 3 times, and 1.5 hours every time, 12 times of amount water of first time simultaneously impregnated 1h, remaining is twice
Add 10 times of amount water, merges No. 3 extracting solutions, macroporous resin column loading (HPD200A macroreticular resin, diameter height ratio 1:7), loading speed≤
2BV/h, loading is complete to be rinsed with water to colourless, is eluted with 6BV55% ethyl alcohol with≤1.5BV/h speed, is concentrated under reduced pressure, recycles second
Alcohol, until density is 1.24g/ml, 60 DEG C are dried under reduced pressure, and are crushed, are obtained extract 3.
3 kinds of extracts are uniformly mixed, appropriate microcrystalline cellulose, 4% PVP K30,3% low substitution hydroxyl are added
Propyl cellulose is uniformly mixed, granulation.
Grain made parameter is as follows:
Feeding motor: 8Hz
Tabletting motor: 16Hz
Crush motor: 10Hz
Whole grain motor: 18Hz
After granulation, 1% magnesium stearate is added, three-dimensional mixer mixes, bladder type stamping, and slice weight 0.6g, every quite
In crude drug 3.8g.
It is coated using stomach dissolved film coating pre-mix dose, weight gain 2%.Seed-coating machine parameter is as follows:
Temperature of charge: 40 DEG C~43 DEG C
Inlet air temperature: 78 DEG C
Leaving air temp: 50 DEG C~80 DEG C
Rotation speed of fan: 1000rpm
Atomizing pressure: 2.2MPa.
Embodiment 4: 9 parts of rheum officinale, 15 parts of oriental wormwood, 3 parts of cape jasmine, preparation method are taken are as follows:
Big yellow water refluxing extraction 3 times, each 1.5h, 8 times of amount water, adds 2 times of amounts for the first time, filters, merging filtrate is dense every time
Density 1.12g/ml (60 DEG C) are reduced to, are let cool, are added the ethyl alcohol of 4 times of volumes, alcohol precipitation 24 hours.Alcohol hypostasis is spare, on alcohol precipitation
Ethyl alcohol is recovered under reduced pressure to no alcohol taste (density be 1.12g/ml (60 DEG C)) in clear liquid, is extracted 4 times with the ethyl acetate of 1 times of volume,
Combined ethyl acetate layer extract liquor obtains gallic acid position after recycling ethyl acetate, is uniformly mixed with alcohol hypostasis, depressurize (60 DEG C)
It dry, pulverize, obtain extract 1.
75% ethyl alcohol of capillary wormwood extracts 2 times, 1 hour every time, adds 10 times of amount solvents for the first time and impregnates 2h, and second plus 8
Times amount solvent, combined extract are concentrated under reduced pressure, and recycling ethyl alcohol is diluted with water to density as 0.1g crude drug/ml to no alcohol taste, and 200
The filtering of mesh gauze, stands, and takes supernatant loading HPD200A macroporous resin column, loading speed≤1BV/h, and the complete water of loading rinses
1BV elutes 3BV with 50% ethyl alcohol with≤1BV/h speed, collects eluent, and it is 1.25g/ml that 60 DEG C, which are concentrated under reduced pressure into density, and 60
It DEG C is dried under reduced pressure, crushes, obtain extract 2.
Cape jasmine is ground into coarse powder, and water extracts 3 times, and 1 hour every time, 14 times of amount water of first time simultaneously impregnated 2h, remaining adds twice
10 times of amount water, merge No. 3 extracting solutions, macroporous resin column loading (HPD200A macroreticular resin, diameter height ratio 1:7), and loading speed≤
3BV/h, loading is complete to be rinsed with water to colourless, is eluted with 5BV50% ethyl alcohol with≤3BV/h speed, is concentrated under reduced pressure, recycles ethyl alcohol,
It is 1.25g/ml to density, 60 DEG C are dried under reduced pressure, and crush, obtain extract 3.
3 kinds of extracts are uniformly mixed, appropriate microcrystalline cellulose, 5% PVP K30,3% low substitution hydroxyl are added
Propyl cellulose is uniformly mixed, granulation.
Grain made parameter is as follows:
Feeding motor: 8Hz
Tabletting motor: 18Hz
Crush motor: 10Hz
Whole grain motor: 18Hz
After granulation, 1% magnesium stearate is added, three-dimensional mixer mixes, bladder type stamping, and slice weight 0.6g, every quite
In crude drug 3.8g.
It is coated using stomach dissolved film coating pre-mix dose, weight gain 3%.Seed-coating machine parameter is as follows:
Temperature of charge: 40 DEG C~43 DEG C
Inlet air temperature: 83 DEG C
Leaving air temp: 50 DEG C~80 DEG C
Rotation speed of fan: 1200rpm
Atomizing pressure: 2.5MPa.
Embodiment 5: preparation process is investigated
(1) selection of granulating process
According to tablet producing technology characteristic combination recipe quantity, since raw material is powder, extract specific gravity is larger, and auxiliary material is empty
The area of a room is narrow, intends selection granulation technique and improves material fluidity, in favor of tabletting；Pass through wet granulation and dry granulation method ratio
Compared with containing water soluble ingredient such as polysaccharide etc. in mixed extract, hygroscopicity is larger, wet granulation sieve easy to stick, not easily molded.Cause
This has selected dry granulation, while adding adhesive PVP K30.Pass through filler microcrystalline cellulose MCC and bonding in auxiliary material
The ratio of agent PVP K30, which compares, to be investigated, the results showed that the ratio of 75% ︰ 25% can make material have preferable stream
Dynamic property.
1. granulating process of table investigates result
Filler and adhesive ratio are investigated in 2. auxiliary material of table
| Filler MCC and adhesive K30 ratio | 50% ︰ 50% | 75% ︰ 25% | 100% ︰ 0% |
| Angle of repose | 41° | 47° | 37° |
(2) selection of auxiliary material: in order to make active component that there is better bioavilability, better formulation properties, intend choosing
The investigations condition such as supplementary product kind, supplementary product consumption is selected, using the disintegration time limited of tablet as index, investigates supplementary product kind and dosage.Finally
Select that microcrystalline cellulose is appropriate, 5% PVP K30,3% low-substituted hydroxypropyl cellulose is as granulation auxiliary material.
Meanwhile to guarantee that the tablet surface of compacting is smooth, sticking is avoided, the magnesium stearate lubricant that 1% is added after granulation carries out tabletting.
Disintegration time limited comparison before and after disintegrating agent is added in table 3.
| Not plus disintegrating agent (n=6) | 3% low-substituted hydroxypropyl cellulose (n=6) | 3% carboxyrnethyl starch sodium (n=6) | |
| Disintegration time > 1h | 3 | 0 | 0 |
| Disintegration time>0.5h,<1h | 3 | 0 | 3 |
| Disintegration time < 0.5h | 0 | 6 | 3 |
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.And these
Belong to the obvious changes or variations that connotation of the invention is extended out and still falls within protection scope of the present invention.
Claims (7)
1. a kind of preparation method of Artemisia capillaris piece, Artemisia capillaris piece is prepared by rheum officinale, oriental wormwood, Fructus Gardeniae extraction, feature
It is, this method comprises the steps of: (1) rheum officinale water extract-alcohol precipitation, supernatant concentration, ethyl acetate extraction concentration, with alcohol precipitation
Drying is precipitated, Chinese rhubarb extract dry cream is obtained；(2) oriental wormwood is extracted with ethyl alcohol, macroporous resin purification, dry, and it is dry to obtain capillary extract
Cream；(3) cape jasmine is extracted with water, macroporous resin purification, dry, obtains capejasmine extract dry cream；(4) be prepared three kinds are extracted
Object dry cream and auxiliary material mixing, granulation；(5) tabletting；(6) it is coated.
2. preparation method as claimed in claim 1, which is characterized in that big yellow water described in step (1) extracts 3 times, and 1.5 is small every time
When, add 10 times of amount water for the first time, remaining adds 8 times of amount water, combined extract twice, and relative density when being concentrated into 60 DEG C is
1.10-1.15 is let cool to room temperature, adds 4 times of 95% ethyl alcohol of amount, stands 24 hours, precipitate it is spare, when supernatant is concentrated into 60 DEG C
Relative density is 1.10-1.15, is extracted 4 times with isometric ethyl acetate, obtains after taking ethyl acetate layer to recycle ethyl acetate and does not eat
Sub- acid position, precipitates combination drying with alcohol precipitation.
3. preparation method as claimed in claim 1, which is characterized in that the 75% ethyl alcohol extraction 2 times of oriental wormwood described in step (2), often
Secondary 1 hour, adding 12 times of amount solvents for the first time and impregnate 2h, second plus 8 times of amount solvents merge No. 2 extracting solutions, are concentrated under reduced pressure,
Ethyl alcohol is recycled to no alcohol taste, being diluted with water to density is 0.1g crude drug/ml, and the filtering of 200 mesh gauzes stands, takes supernatant loading
HPD200A macroporous resin column, loading speed≤1BV/h, the complete water of loading rinse 1BV, with 50% ethyl alcohol with≤1BV/h speed elution
3BV collects eluent, and it is 1.22-1.26g/ml that 60 DEG C, which are concentrated under reduced pressure into density, and 60 DEG C are dried under reduced pressure, and is crushed.
4. preparation method as claimed in claim 1, which is characterized in that cape jasmine described in step (3) is extracted with water, and cape jasmine is ground into slightly
Powder, water extract 3 times, and 1 hour every time, 14 times of amount water of first time simultaneously impregnated 2h, remaining adds 10 times of amount water twice, merged 3 extractions
Liquid, macroporous resin column loading HPD200A macroreticular resin, diameter height ratio 1:7, loading speed≤3BV/h, loading is complete to be rinsed with water to nothing
Color is eluted with≤3BV/h speed with 5BV50% ethyl alcohol, is concentrated under reduced pressure, recycles ethyl alcohol, until density is 1.22-1.26g/ml, 60
It DEG C is dried under reduced pressure, crushes.
5. preparation method as claimed in claim 1, which is characterized in that 3 extract dry cream mixing described in step (4) are added micro-
Crystalline cellulose, PVP K30, low substituted hydroxy-propyl fiber, dry granulation, dry granulation technology use following technique
Parameter: feeding motor: 4~12Hz；Tabletting motor: 12~22Hz；Crush motor: 5~15Hz；Whole grain motor: 12~22Hz.
6. preparation method as claimed in claim 1, which is characterized in that step (6) coating, seed-coating machine parameter are as follows: temperature of charge: 40
DEG C~43 DEG C；Inlet air temperature: 70 DEG C~83 DEG C；Leaving air temp: 50 DEG C~80 DEG C；Rotation speed of fan: 800~1200rpm；Atomization pressure
Power: 1.5~3 MPa.
7. preparation method as claimed in claim 1, which is characterized in that Artemisia capillaris piece is prepared by following parts by weight medicinal material extract:
5~9 parts of rheum officinale, 12~15 parts of oriental wormwood, 3~9 parts of cape jasmine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910474673.3A CN110090251B (en) | 2019-06-03 | 2019-06-03 | Preparation method of artemisia capillaris tablet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910474673.3A CN110090251B (en) | 2019-06-03 | 2019-06-03 | Preparation method of artemisia capillaris tablet |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110090251A true CN110090251A (en) | 2019-08-06 |
| CN110090251B CN110090251B (en) | 2021-07-06 |
Family
ID=67450039
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910474673.3A Active CN110090251B (en) | 2019-06-03 | 2019-06-03 | Preparation method of artemisia capillaris tablet |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110090251B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101371882A (en) * | 2007-08-24 | 2009-02-25 | 曾雄辉 | Method for preparing Artemisia capillaris decoction formulation |
| CN101407532A (en) * | 2008-11-24 | 2009-04-15 | 浙江省中药研究所有限公司 | Method for preparing gardenin from gardenia |
| CN101940642A (en) * | 2010-10-08 | 2011-01-12 | 华东理工大学 | Chinese medicinal composition and application thereof |
| CN102309579A (en) * | 2011-09-16 | 2012-01-11 | 陕西科技大学 | Tarragon soup effervescent tablet and its preparation method |
-
2019
- 2019-06-03 CN CN201910474673.3A patent/CN110090251B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101371882A (en) * | 2007-08-24 | 2009-02-25 | 曾雄辉 | Method for preparing Artemisia capillaris decoction formulation |
| CN101407532A (en) * | 2008-11-24 | 2009-04-15 | 浙江省中药研究所有限公司 | Method for preparing gardenin from gardenia |
| CN101940642A (en) * | 2010-10-08 | 2011-01-12 | 华东理工大学 | Chinese medicinal composition and application thereof |
| CN102309579A (en) * | 2011-09-16 | 2012-01-11 | 陕西科技大学 | Tarragon soup effervescent tablet and its preparation method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110090251B (en) | 2021-07-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102940695B (en) | Medicine composition for treating gout | |
| CN103655791B (en) | A kind of lotus leaf-based preparation for treating phlegm and blood stasis simultaneously and application thereof | |
| CN108434399A (en) | A kind of Chinese medicine composition and preparation method of anti-curing oncoma | |
| CN102961584B (en) | Traditional Chinese medicine composition capable of relieving fatigue, as well as preparation method and application thereof | |
| CN110090251A (en) | A kind of preparation method of Artemisia capillaris piece | |
| CN102940709B (en) | Medicine composition for treating gout | |
| CN1839981A (en) | Gynecological inflammation resisting dispersion tablet and its preparation method | |
| CN101091774A (en) | Composition of Chinese traditional medicine for treating diabetes, and preparation method | |
| CN102920964A (en) | Traditional Chinese medicine preparation for curing cough | |
| CN102940750B (en) | Medicine composition for treating gout | |
| CN103316092A (en) | Preparation technology of Jindan tablets | |
| CN101057894B (en) | Traditional Chinese medicine preparation for curing gynecologic and its preparation method | |
| CN100402073C (en) | Medicine for treating disease caused by heat toxin | |
| CN103599343A (en) | Pharmaceutical composition for treating diabetes, and preparation method and application thereof | |
| CN102940747B (en) | Medicine composition for treating gout | |
| CN101049463B (en) | Preparation of Chinese traditional medicine in use for hepatic disease and preparation method | |
| CN111329966A (en) | Traditional Chinese medicine composition for treating skin itch and extract and preparation thereof | |
| CN107625894A (en) | A kind of preparation method of compound ginseng stilbene dispersible tablet | |
| CN102764319A (en) | Traditional Chinese medicine vagina effervescent tablets for curing cervical erosion of women and preparation method thereof | |
| CN108743771A (en) | A kind of Fuke Tiaojing tablets and its preparation process | |
| CN110420264B (en) | Traditional Chinese medicine composition and preparation method and application thereof | |
| CN1285379C (en) | Recipe composition of cold-resisting Chinese medicine sugar-less granular powder and tablet and preparing process | |
| CN103055018A (en) | Freeze-dried fresh rehmannia for treating senile dementia | |
| CN104398564A (en) | Tripterygium wilfordii containing Chinese medicinal composition for treatment of gout | |
| CN101194966B (en) | Buccal tablets for treating headache and method for preparing the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |