CN109985100A - A kind of preparation method and its method of quality control of Chinese knotweed's granule - Google Patents

A kind of preparation method and its method of quality control of Chinese knotweed's granule Download PDF

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CN109985100A
CN109985100A CN201910263857.5A CN201910263857A CN109985100A CN 109985100 A CN109985100 A CN 109985100A CN 201910263857 A CN201910263857 A CN 201910263857A CN 109985100 A CN109985100 A CN 109985100A
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China
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chinese knotweed
granule
chinese
knotweed
quality control
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朱月信
陈培胜
成守玲
孟繁民
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ANHUI JIREN PHARMACEUTICAL Co Ltd
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ANHUI JIREN PHARMACEUTICAL Co Ltd
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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)
    • A61K36/70—Polygonaceae (Buckwheat family), e.g. spineflower or dock
    • A61K36/704—Polygonum, e.g. knotweed
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605—Excipients; Inactive ingredients
    • A61K9/1629—Organic macromolecular compounds
    • A61K9/1652—Polysaccharides, e.g. alginate, cellulose derivatives; Cyclodextrin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
    • A61P1/12—Antidiarrhoeals
    • 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
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P11/00—Drugs for disorders of the respiratory system
    • A61P11/04—Drugs for disorders of the respiratory system for throat disorders
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
    • G01N30/95—Detectors specially adapted therefor; Signal analysis
    • 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
    • A61K2236/39—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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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Animal Behavior & Ethology (AREA)
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  • Pharmacology & Pharmacy (AREA)
  • Bioinformatics & Cheminformatics (AREA)
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Abstract

The invention discloses the preparation methods and its method of quality control of a kind of Chinese knotweed's granule, the granule is using Chinese knotweed's medicine materical crude slice as raw material, by water extract twice, reduceds pressure, spray drying, the obtained Chinese knotweed's granule of the process flows such as dry granulation, every gram of Chinese knotweed's granule 16-17 grams of crude drug amount suitable, and Chinese knotweed's granule carries out quality discrimination using thin-layer chromatography.The present invention is on the basis of motherland's Chinese Traditional Medicine decoction, in conjunction with modern high technology extract equipment, pharmaceutical technology and thin layer scanning technology, and refer to Chinese knotweed's chemical constitution study, technical study, TLC Identification research are extracted to Chinese knotweed, the Chinese knotweed's granule taken can directly be dissolved before use by obtaining one kind.The medicine can be realized full constituents extraction, Manufacturing science, quality controllable, may be implemented to be mass produced.The medical instrument have it is convenient to take, health, convenient for storage.

Description

A kind of preparation method and its method of quality control of Chinese knotweed's granule
Technical field
The present invention relates to the preparation method of traditional Chinese medicine product technical field more particularly to a kind of Chinese knotweed's granule and its Method of quality control.
Background technique
Chinese knotweed, nature and flavor are sour, sweet, cold, have the effect of clearing heat and promoting diuresis, removing pattogenic heat from the blood and toxic material from the body, for being used for diarrhea due to damp-heat, dysentery Disease, jaundice, abscess of throat.
Chinese knotweed is used as medicine with medicine materical crude slice, and the mode of decoction taken, The Quality of Sliced Herbal Medicine are unstable not before use Controllably, it decocts quality to be difficult to ensure, takes inconvenience, be not easy to store.And Chinese medicinal granule is to meet the excellent of concocted specification Matter medicinal material (prepared slices of Chinese crude drugs) is raw material, is extracted, is concentrated using modern high technology, product system class made of granulation, guaranteed original The nature and flavor feature of Chinese medicine.There is presently no unified standard, each manufacturer is all that production and quality control are carried out with company standard System, causes Chinese knotweed's granule quality irregular.
Summary of the invention
The object of the invention is to remedy the disadvantages of known techniques, provides a kind of preparation method of Chinese knotweed's granule And its method of quality control.
The present invention is achieved by the following technical solutions:
A kind of preparation method of Chinese knotweed's granule, comprising the following steps:
(1) Chinese knotweed's medicine materical crude slice is put into extractor, decocted twice, add the water of 7-9 times of medicine materical crude slice amount for the first time, it is small that heating decocts 1-2 When, second plus 6-8 times of water of medicine materical crude slice amount decoct 1-2 hours, and medical fluid filtration, filtrate merges, and filtrate is pumped into concentration tank, is concentrated into Relative density is the medicinal extract of 1.07-1.09, crosses 150-200 mesh while hot, spare；
(2) step 1 gained medicinal extract is taken, the maltodextrin of Chinese knotweed's medicine materical crude slice amount 2-3% is added, mixes, is heated to 70-80 DEG C, it is spraying It is dry, dried cream powder is collected, it is spare；
(3) step 2 gained dried cream powder is crushed, crosses 80-120 mesh；Dry granulation, with medicinal composite film packaging, pack to get Finished product.
Described every gram of Chinese knotweed's granule is equivalent to 16-17 grams of crude drug amount.
Preferably, 16.7 grams of crude drug amount are equivalent to for described every gram of Chinese knotweed's granule.
A kind of method of quality control of Chinese knotweed's granule indentification by TLC as obtained by the above method, including following step It is rapid:
(1) Chinese knotweed granule powder 1g is taken, adds methanol 20ml, refluxing extraction 2 hours, filtration, filtrate was evaporated, and residue adds second Ether 20ml dissolution, shaking extract 30 minutes, ether extracted liquid is evaporated, residue add diethyl ether 2ml dissolution, it is standby as test solution With；
(2) it takes Chinese knotweed to coarse powder 5g, adds water 50ml, boil 40 minutes, filter, filtrate is evaporated, and residue adds methanol 20ml, synchronous Rapid 1 is made contrast solution, spare；
(3) it is tested using thin-layered chromatography, draws test solution, each 10 μ l of Chinese knotweed's contrast solution, put respectively in same silicon Glue GF254On lamellae, using toluene-ethyl acetate-formic acid as solvent, expansion；
(4) it will be taken out by the lamellae after the expansion of step 3 method, dry, set inspected under ultraviolet lamp 254nm, 365nm respectively, In sample chromatogram, on position corresponding with contrast solution chromatography, the spot or fluorescence spot of same color should be shown.
Contain 1ml hydrochloric acid in methanol in the step 1 and 2.
Toluene-ethyl acetate-formic acid volume ratio is 5:4:1 in the step 3.
The invention has the advantages that
The present invention is on the basis of motherland's Chinese Traditional Medicine decoction, in conjunction with modern high technology extract equipment, pharmaceutical technology and thin layer Scanning technique, and Chinese knotweed's chemical constitution study is referred to, technical study is extracted to Chinese knotweed, TLC Identification is ground Study carefully, the Chinese knotweed's granule taken can directly be dissolved before use by obtaining one kind.The medicine can be realized full constituents extraction, raw It is obstetrics, quality controllable, it may be implemented to be mass produced.The medical instrument have it is convenient to take, health, convenient for storage.
Detailed description of the invention
Fig. 1 show Chinese knotweed's granule of the present invention thin-layer chromatogram at 254nm and 365nm respectively, wherein 1-3 For test sample, 4-6 is Chinese knotweed's control.
Specific embodiment
Below in conjunction with specific example, technical scheme is described further:
Embodiment 1
The preparation of Chinese knotweed's granule:
(1) raw material is weighed: Chinese knotweed's medicine materical crude slice 5760g；
(2) Chinese knotweed's medicine materical crude slice is put into extractor, decocted twice, added 8 times of medicine materical crude slice amount of water for the first time, decoct 1 hour, second Add 7 times of water of medicine materical crude slice amount, decoct 1 hour, medical fluid filtration, filtrate merges, and is pumped into concentration tank, (steam pressure is in 0.04- for concentration Between 0.09Mpa, vacuum degree -0.04~-0.08MPa), being concentrated into relative density is 1.07-1.09(80 DEG C) medicinal extract, take advantage of Heat crosses 200 meshes, spare；
(3) step 2 gained medicinal extract is taken, maltodextrin 0.17g is added, is mixed, is heated to 70 DEG C, spray drying (control air inlet temperature 175-185 DEG C of degree, 85-95 DEG C of leaving air temp), dried cream powder is collected, it is spare；
(4) step 3 gained dried cream powder is crushed, crosses 80 meshes；Dry granulation (adjusts principal pressure 20-40MPa, lateral pressure 10MPa, by roll rotational speed 12-25Hz), with medicinal composite film packaging (0.9g/ bags of loading amount) to get finished product.
Embodiment 2
The method of quality control of Chinese knotweed's granule indentification by TLC:
(1) Chinese knotweed granule powder 1g is taken, methanol 20ml(is added to include 1ml hydrochloric acid), refluxing extraction 2 hours, filtration, filtrate Be evaporated, residue add diethyl ether 20ml dissolution, shaking extract 30 minutes, ether extracted liquid is evaporated, residue add diethyl ether 2ml dissolution, as Test solution, it is spare；
(2) it takes Chinese knotweed to coarse powder 5g, adds water 50ml, boil 40 minutes, filter, filtrate is evaporated, and residue adds methanol 20ml(to include 1ml hydrochloric acid), contrast solution is made with step 1, it is spare；
(3) referring to four 0502 thin-layered chromatography of the general rule tests of " Chinese Pharmacopoeia " version in 2015, test solution, Chinese knotweed are drawn Each 10 μ l of contrast solution, puts respectively in same silica G F254It is expansion with toluene-ethyl acetate-formic acid (5:4:1) on lamellae Agent, expansion；
(4) lamellae after the expansion of step 3 method is taken out, dries, sets inspected under ultraviolet lamp 254nm, 365nm respectively.For In test product chromatography, on position corresponding with contrast solution chromatography, the spot or fluorescence spot of same color are shown, as shown in Figure 1, Show to contain Chinese knotweed's ingredient in test sample.
Embodiment 3
Moisture, granularity, melting, content uniformity and determination of extractives in Chinese knotweed's granule:
To the moisture in Chinese knotweed's granule finished product of 6 batches prepared in aforementioned manners, granularity, melting, extract It is detected.Moisture, melting, content uniformity are detected according to a conventional method.Determination of extractives is surveyed according to ethanol soluble extractives Hot dipping (four general rules 2201 of " Chinese Pharmacopoeia " version in the 2015) measurement under method item is determined, with 70% ethanol as solvent.Items check The results are shown in Table 1, shows that indices comply with standard.
The every testing result of table 1
Lot number Moisture Melting Content uniformity Granularity Extract
1 3.1 It is qualified It is qualified It is qualified 42.1
2 3.3 It is qualified It is qualified It is qualified 47.0
3 4.0 It is qualified It is qualified It is qualified 39.4
4 3.5 It is qualified It is qualified It is qualified 39.2
5 4.0 It is qualified It is qualified It is qualified 44.5
6 3.6 It is qualified It is qualified It is qualified 40.5

Claims (6)

1. a kind of preparation method of Chinese knotweed's granule, which comprises the following steps:
(1) Chinese knotweed's medicine materical crude slice is put into extractor, decocted twice, add the water of 7-9 times of medicine materical crude slice amount for the first time, it is small that heating decocts 1-2 When, second plus 6-8 times of water of medicine materical crude slice amount decoct 1-2 hours, and medical fluid filtration, filtrate merges, and filtrate is pumped into concentration tank, is concentrated into Relative density is the medicinal extract of 1.07-1.09, crosses 150-200 mesh while hot, spare；
(2) step 1 gained medicinal extract is taken, the maltodextrin of Chinese knotweed's medicine materical crude slice amount 2-3% is added, mixes, is heated to 70-80 DEG C, it is spraying It is dry, dried cream powder is collected, it is spare；
(3) step 2 gained dried cream powder is crushed, crosses 80-120 mesh；Dry granulation, with medicinal composite film packaging, pack to get Finished product.
2. the preparation method of Chinese knotweed's granule according to claim 1, which is characterized in that Chinese knotweed's formula Every gram of grain is equivalent to 16-17 grams of crude drug amount.
3. the preparation method of Chinese knotweed's granule according to claim 1, which is characterized in that Chinese knotweed's formula Every gram of grain is equivalent to 16.7 grams of crude drug amount.
4. a kind of method of quality control of such as claim 1 gained Chinese knotweed granule indentification by TLC, which is characterized in that The following steps are included:
(1) Chinese knotweed granule powder 1g is taken, adds methanol 20ml, refluxing extraction 2 hours, filtration, filtrate was evaporated, and residue adds second Ether 20ml dissolution, shaking extract 30 minutes, ether extracted liquid is evaporated, residue add diethyl ether 2ml dissolution, it is standby as test solution With；
(2) it takes Chinese knotweed to coarse powder 5g, adds water 50ml, boil 40 minutes, filter, filtrate is evaporated, and residue adds methanol 20ml, synchronous Rapid 1 is made contrast solution, spare；
(3) it is tested using thin-layered chromatography, draws test solution, each 10 μ l of Chinese knotweed's contrast solution, put respectively in same silicon Glue GF254On lamellae, using toluene-ethyl acetate-formic acid as solvent, expansion；
(4) it will be taken out by the lamellae after the expansion of step 3 method, dry, set inspected under ultraviolet lamp 254nm, 365nm respectively, In sample chromatogram, on position corresponding with contrast solution chromatography, the spot or fluorescence spot of same color should be shown.
5. method of quality control according to claim 4, which is characterized in that contain in the methanol in the step 1 and 2 1ml hydrochloric acid.
6. method of quality control according to claim 4, which is characterized in that toluene-ethyl acetate-first in the step 3 The volume ratio of acid is 5:4:1.
CN201910263857.5A 2019-04-03 2019-04-03 A kind of preparation method and its method of quality control of Chinese knotweed's granule Withdrawn CN109985100A (en)

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CN201910263857.5A CN109985100A (en) 2019-04-03 2019-04-03 A kind of preparation method and its method of quality control of Chinese knotweed's granule

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Application publication date: 20190709