CN104288194B - A kind of preparation method of compound isatis root granules - Google Patents

A kind of preparation method of compound isatis root granules Download PDF

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CN104288194B
CN104288194B CN201410596822.0A CN201410596822A CN104288194B CN 104288194 B CN104288194 B CN 104288194B CN 201410596822 A CN201410596822 A CN 201410596822A CN 104288194 B CN104288194 B CN 104288194B
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concentrated
relative density
temperature
ethanol
cellulase
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CN104288194A (en
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黄琴
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Guangdong Xiangshantang Pharmaceutical Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/19Acanthaceae (Acanthus family)
    • A61K36/195Strobilanthes
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/31Brassicaceae or Cruciferae (Mustard family), e.g. broccoli, cabbage or kohlrabi
    • A61K36/315Isatis, e.g. Dyer's woad
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605Excipients; Inactive ingredients
    • A61K9/1629Organic macromolecular compounds
    • A61K9/1652Polysaccharides, e.g. alginate, cellulose derivatives; Cyclodextrin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/19Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331Extraction 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
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/55Liquid-liquid separation; Phase separation

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  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Chemical & Material Sciences (AREA)
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  • General Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Animal Behavior & Ethology (AREA)
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  • Alternative & Traditional Medicine (AREA)
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Abstract

The invention discloses a kind of preparation method of compound isatis root granules, comprise the following steps:By Radix Isatidis raw material, secondary, 2 hours for the first time, second 1 hour, collecting decoction, filtration are added water to cook;2) it is 1.10 that filtrate, which is concentrated into relative density, and temperature 45 C adds pectase, cellulase, the complex enzyme of the composition of pectin lyase and digested, pectase, cellulase, the weight ratio of pectin lyase are 5:3:2, complex enzyme addition is 0.5 1.0% of filtrate weight after concentrating;It is 1.20 to continue to be concentrated into relative density, and temperature 45 C is filtered, cooling, and adding 95% ethanol makes alcohol content be 30%, and quiescent setting extracts supernatant;Ethanol is reclaimed, it is 1.20 that relative density is concentrated into when temperature is 70 DEG C;The sucrose and dextrin of conventional amount used are added, particle is made, is dried.The present invention is by adding enzymolysis process, it is possible to reduce concentration of alcohol during alcohol precipitation, reduces cost.

Description

A kind of preparation method of compound isatis root granules
Technical field
The present invention relates to a kind of preparation method of medicine, and in particular to a kind of preparation method of compound isatis root granules.
Background technology
Radix Isatidis (conventional alias:Indigo-blue, indigo root, manyflower glorybower root) it is a kind of Chinese medicine.Produce all over China.Radix Isatidis Be divided into northern Radix Isatidis and rhizoma et Radix Baphicacanthis Cusiae, northern Radix Isatidis source for cruciferae isatis (Isatis tinctoria L.) and The root of careless smalt (I.indigotica Fort.);Rhizoma et Radix Baphicacanthis Cusiae is acanthaceous vegetable acanthaceous indigo (Baphicacanthus cusia (Nees) Brem.) rhizome and root, the effect of with clearing heat and detoxicating, preventing cold, relieving sore-throat.Cure mainly:Febrile virulent maculae, hyperpyrexia head Bitterly, major part pestilence, tongue dark reddish purple dark, scarlet fever, erysipelas, mumps, larynx numbness, sore swells, carbuncle swells, varicella, measles, hepatitis, popularity Flu, epidemic meningitis, encephalitis, pneumonia, coma hematemesis, pharynx swelling, pinkeye, sore rash;Can prevent and treat Japanese Type-B encephalitis, acute, chronic hepatitis, Mumps, osteomyelitis.
Compound isatis root granules, main component is Radix Isatidis, and auxiliary material is sucrose, and dextrin is the particle of brown or sepia; Taste sweet tea, slight bitter.Mainly there are two kinds of sugar-containing type and Sugarless type.Compound isatis root granules, clearing heat and detoxicating, cool blood, for anemopyretic cold, Abscess of throat.Radix Isatidis is taken during flu, is conducive to enhancing immune, virus and pathogenic bacteria in vivo is killed, is conducive to rehabilitation;Stream During sense and Radix Isatidis is taken during viral disease, is conducive to building up resistance, it is to avoid is infected.For caused by lung and stomach excessive heat Abscess of throat, pharyngoxerosis, acute tonsillitis.
At present, the preparation method of compound isatis root granules is:By Radix Isatidis 1400g, add water to cook it is secondary, it is 2 small for the first time When, second 1 hour, collecting decoction, filtration, filtrate was concentrated into relative density for 1.20 (50 DEG C), plus ethanol makes the alcohol content be 60%, standing makes precipitation, takes supernatant, reclaims ethanol and is concentrated into appropriate.Thick paste is taken, appropriate sucrose and dextrin, system is added Into particle, dry, 1000g is made;Or thick paste is taken, appropriate dextrin and sweetener is added, particle is made, dries, 600g is made (Sugarless type), is produced.Such preparation method comes with some shortcomings, and drops to room temperature as decoction must be placed to temperature and could add Ethanol, but due to the gelatinization of starch, decoction is changed into g., jelly-like, is difficult now to enter ethanol to be dissolved with inside g., jelly-like thing Composition is imitated, while being deposited the gelatinized starch got off has wrapped up active ingredient, there is that ethanol consumption is big, active ingredient is easily wrapped Precipitation causes the shortcoming of yield reduction.
In summary, the optimization to the preparation method of existing compound isatis root granules is necessary.
The content of the invention
The technical problem to be solved in the present invention is in view of the shortcomings of the prior art, to the preparation method of compound isatis root granules Optimize, improve production efficiency, reduce cost.
In order to solve the above technical problems, the technical solution adopted by the present invention is:
1) by Radix Isatidis raw material, secondary, 2 hours for the first time, second 1 hour, collecting decoction, filtration are added water to cook;
2) filtrate is concentrated into relative density for 1.10, temperature 45 C, adds pectase, cellulase, pectin lyase The complex enzyme of composition is digested, and pectase, cellulase, the weight ratio of pectin lyase are 5:3:2, complex enzyme addition is The 0.5-1.0% of filtrate weight after concentration;
3) it is 1.20 to continue to be concentrated into relative density, and temperature 45 C is filtered, cooling, and adding 95% ethanol makes the alcohol content be 30%, quiescent setting extracts supernatant;
4) ethanol is reclaimed, it is 1.20 that relative density is concentrated into when temperature is 70 DEG C;
5) sucrose and dextrin of conventional amount used are added, particle is made, is dried.
It is of the present invention to decoct, using prior art common process.
Compared with prior art, the present invention has advantages below:
1st, water extraction and alcohol precipitation method is the Hydrolysis kinetics method commonly used during Chinese medicine preparation is produced.Concentration of alcohol is solid to Chinese medicine during alcohol precipitation Body preparation curative effect, taking dose, dosage form selection, preparations shaping, product stability etc. have a major impact, second during reasonable selection alcohol precipitation Determining alcohol is one of key link during solid preparation of traditional Chinese medicine.However, at present in the research of water extraction and alcohol precipitation method alcohol precipitation process, General main examination alcohol precipitation process influence factor, such as relative density of traditional Chinese medicine extraction concentrated liquor, alcohol precipitation temperature, the alcohol precipitation time and Plus alcohol mode etc. is to traditional Chinese medicinal ointment index components content, the influence of yield of extract, seldom research alcohol precipitation when ethanol consumption to whole system The influence of agent process etc., often brings problem to follow-up production process and preparation stability.The present invention by adding enzymolysis process, Concentration of alcohol during alcohol precipitation can be reduced, cost is reduced.
2nd, amylase is added when prior art has research using leaching process, but because starch is from the leaching of medicinal material organization internal Profit-dissolving-diffusion process is far longer than the inactivation speed of amylase, causes effect to control.Somebody's research uses 80 DEG C Soak extraction Radix Isatidis extractum, although greatly reduce the leaching of starch, but also greatly reduce the leaching of active ingredient simultaneously, Cause the waste of herb resource.Carbohydrate (polysaccharide, oligosaccharides), adenosine, organic acid, amino acids, life are mainly contained in Radix Isatidis The compounds such as alkaloids class, and the present invention, compared to single enzyme, is targetedly worked by the application to complex enzyme, can be compared with Decompose polysaccharose substance well, it is to avoid above drawback, effect is obvious.
3rd, by the process optimization of the present invention, to the Radix Isatidis index components adenosine rate of transform, yield of extract, and to spraying Drying process, medicinal extract dry jet mixing pile, moulding process all bring larger improvement.
Embodiment
With embodiment, the invention will be further described below, but the invention is not limited in these embodiments.
Embodiment 1:
1) by Radix Isatidis raw material, secondary, 2 hours for the first time, second 1 hour, collecting decoction, filtration are added water to cook;
2) filtrate is concentrated into relative density for 1.10, temperature 45 C, adds pectase, cellulase, pectin lyase The complex enzyme of composition is digested, and pectase, cellulase, the weight ratio of pectin lyase are 5:3:2, complex enzyme addition is The 0.5% of filtrate weight after concentration;
3) it is 1.20 to continue to be concentrated into relative density, and temperature 45 C is filtered, cooling, and adding 95% ethanol makes the alcohol content be 30%, quiescent setting extracts supernatant;
4) ethanol is reclaimed, it is 1.20 that relative density is concentrated into when temperature is 70 DEG C;
5) sucrose and dextrin of conventional amount used are added, particle is made, is dried.
Embodiment 2:
1) by Radix Isatidis raw material, secondary, 2 hours for the first time, second 1 hour, collecting decoction, filtration are added water to cook;
2) filtrate is concentrated into relative density for 1.10, temperature 45 C, adds pectase, cellulase, pectin lyase The complex enzyme of composition is digested, and pectase, cellulase, the weight ratio of pectin lyase are 5:3:2, complex enzyme addition is The 1.0% of filtrate weight after concentration;
3) it is 1.20 to continue to be concentrated into relative density, and temperature 45 C is filtered, cooling, and adding 95% ethanol makes the alcohol content be 30%, quiescent setting extracts supernatant;
4) ethanol is reclaimed, it is 1.20 that relative density is concentrated into when temperature is 70 DEG C;
5) sucrose and dextrin of conventional amount used are added, particle is made, is dried.
Embodiment 3:
1) by Radix Isatidis raw material, secondary, 2 hours for the first time, second 1 hour, collecting decoction, filtration are added water to cook;
2) filtrate is concentrated into relative density for 1.10, temperature 45 C, adds pectase, cellulase, pectin lyase The complex enzyme of composition is digested, and pectase, cellulase, the weight ratio of pectin lyase are 5:3:2, complex enzyme addition is The 0.8% of filtrate weight after concentration;
3) it is 1.20 to continue to be concentrated into relative density, and temperature 45 C is filtered, cooling, and adding 95% ethanol makes the alcohol content be 30%, quiescent setting extracts supernatant;
4) ethanol is reclaimed, it is 1.20 that relative density is concentrated into when temperature is 70 DEG C;
5) sucrose and dextrin of conventional amount used are added, particle is made, is dried.
Comparative example 1:
By Radix Isatidis medicine materical crude slice, secondary, 2 hours for the first time, second 1 hour, collecting decoction, filtration, filtrate are added water to cook Relative density is concentrated into for 1.20 (50 DEG C), plus ethanol makes alcohol content be 60%, standing makes precipitation, takes supernatant, reclaims ethanol And be concentrated into appropriate.Thick paste is taken, appropriate sucrose and dextrin is added, particle is made, is dried.
Comparative example 2:
1) by Radix Isatidis raw material, secondary, 2 hours for the first time, second 1 hour, collecting decoction, filtration are added water to cook;
2) it is 1.10 that filtrate, which is concentrated into relative density, temperature 45 C, adds amylase, and amylase addition is filter after concentration The 0.8% of liquid weight;
3) it is 1.20 to continue to be concentrated into relative density, and temperature 45 C is filtered, cooling, and adding 95% ethanol makes the alcohol content be 50%, quiescent setting extracts supernatant;
4) ethanol is reclaimed, it is 1.20 that relative density is concentrated into when temperature is 70 DEG C;
5) sucrose and dextrin of conventional amount used are added, particle is made, is dried.
Table one:Embodiment and comparative example data statistics
Conclusion:The present invention in Aqueous extracts concentration process by adding complex enzyme, ethanol when can significantly reduce alcohol precipitation Consumption, to the compound isatis root granules obtained by subsequent technique, particle yield, particle friability, the long altar on which incense burners are placed rate of transform with And the spray drying index such as water content all has clear improvement, cost is reduced while quality is improved.

Claims (1)

1. a kind of preparation method of compound isatis root granules, it is characterised in that comprise the following steps:
1) by Radix Isatidis raw material, secondary, 2 hours for the first time, second 1 hour, collecting decoction, filtration are added water to cook;
2) it is 1.10 that filtrate, which is concentrated into relative density, and temperature 45 C adds pectase, cellulase, the composition of pectin lyase Complex enzyme digested, pectase, cellulase, the weight ratio of pectin lyase are 5:3:2, complex enzyme addition is concentration The 0.5-1.0% of filtrate weight afterwards;
3) it is 1.20 to continue to be concentrated into relative density, and temperature 45 C is filtered, cooling, and adding 95% ethanol makes alcohol content be 30%, Quiescent setting, extracts supernatant;
4) ethanol is reclaimed, it is 1.20 that relative density is concentrated into when temperature is 70 DEG C;
5) sucrose and dextrin of conventional amount used are added, particle is made, is dried.
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CN105432899A (en) * 2015-12-31 2016-03-30 桂林双象生物科技有限公司 Preparation method of honeysuckle flower and grosvenor momordica fruit composite tea
CN105477347A (en) * 2015-12-31 2016-04-13 吉林紫鑫药业股份有限公司 Method for preparing medicine used for treating liver-stomach disharmony and blood stasis collateral obstruction
CN106692490A (en) * 2016-12-13 2017-05-24 广西双蚁药业有限公司 Sucrose-free compound isatis root granules and preparation method thereof
CN107349247A (en) * 2017-05-23 2017-11-17 回音必集团安徽制药有限公司 A kind of Radix Isatidis Optimized Extraction Process
CN107582600A (en) * 2017-06-26 2018-01-16 安徽永生堂药业有限责任公司 A kind of banlangen granules, banlangen keli and preparation method thereof
CN107951910A (en) * 2017-12-25 2018-04-24 安徽永生堂药业有限责任公司 A kind of preparation method of compound isatis root granules electuary
CN108969604A (en) * 2018-08-15 2018-12-11 康美保宁(四川)制药有限公司 A kind of pre-treating method and preparation method of compound isatis root granules

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