CN107721962A - A kind of preparation method of baicalein aluminium complex and its preparation - Google Patents
A kind of preparation method of baicalein aluminium complex and its preparation Download PDFInfo
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- CN107721962A CN107721962A CN201710971843.XA CN201710971843A CN107721962A CN 107721962 A CN107721962 A CN 107721962A CN 201710971843 A CN201710971843 A CN 201710971843A CN 107721962 A CN107721962 A CN 107721962A
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- baicalein
- aluminium complex
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
- C07D311/30—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only not hydrogenated in the hetero ring, e.g. flavones
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
- A61K47/08—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing oxygen, e.g. ethers, acetals, ketones, quinones, aldehydes, peroxides
- A61K47/10—Alcohols; Phenols; Salts thereof, e.g. glycerol; Polyethylene glycols [PEG]; Poloxamers; PEG/POE alkyl ethers
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/0087—Galenical forms not covered by A61K9/02 - A61K9/7023
- A61K9/0095—Drinks; Beverages; Syrups; Compositions for reconstitution thereof, e.g. powders or tablets to be dispersed in a glass of water; Veterinary drenches
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/141—Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers
- A61K9/145—Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers with organic compounds
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention belongs to veterinary Chinese medicine preparation technical field, specifically discloses a kind of preparation method of baicalein aluminium complex and its preparation.Baicalein is added to the water, aqueous slkali is added dropwise while stirring, is 6.5 ~ 7 to solution ph；Saturation aluminum contained compound solution is added dropwise while stirring, until stopping addition when no longer producing floccule；Stand overnight, supernatant discarding, and with after aqueous antioxidant solution repeatedly washing precipitate, dry, produce baicalein aluminium complex.The invention provides two kinds of preparation types：Oral liquid and pulvis, aluminium complex containing baicalein 1 ~ 5%.Formulation of the present invention is mainly used in veterinary art, and new direction is provided to develop the animal drug of new type of safe green noresidue.
Description
Technical field
The invention belongs to veterinary Chinese medicine preparation technical field, and in particular to a kind of system of baicalein aluminium complex and its preparation
Preparation Method.
Background technology
Baicalein is flavones ingredient, has adjacent three phenolic hydroxyl groups in chemical constitution, property is very unstable, easily loses biology
Activity, shown by correlative study, can not only improve its stability, and can produce new by forming complex with metal
Pharmacological action.Baicalein aluminium has clearing heat and detoxicating, dampness removing and diarrhea-relieving effect, common dosage forms baicalein aluminium glue capsule, is mainly used in people
The treatment of enteritis and dysentery, clinically therapeutic effect is notable, and without any side effects.But have no in clinical use report for animals
Lead.
The content of the invention
It is an object of the invention to provide the preparation method of a kind of baicalein aluminium complex and its preparation.
To achieve the above object, the technical scheme that the present invention takes is as follows：
A kind of preparation method of baicalein aluminium complex：Baicalein is added to the water, aqueous slkali is added dropwise while stirring, to pH value of solution
It is worth for 6.5 ~ 7；Saturation aluminum contained compound solution is added dropwise while stirring, until stopping addition when no longer producing floccule；Stood
Night, supernatant discarding, and with after aqueous antioxidant solution repeatedly washing precipitate, dry, produce baicalein aluminium complex.
Preferably, the mass ratio of baicalein and water is 1: 30 ~ 40.
Preferably, the aqueous slkali is 2 ~ 3 mol/L NaOH solution or 2 ~ 3 mol/L NaHCO3Solution；It is described full
It is that saturation liquor alumini chloridi, saturation aluminum hydroxide solution, saturation alumina solution, saturation aluminum sulfate are molten with aluminum contained compound solution
Liquid or saturated acetic acid aluminum solutions；The mass concentration of the aqueous antioxidant solution is 0.2 ~ 0.3 %, and the antioxidant is sulfurous
Sour hydrogen sodium, vitamin C or sodium pyrosulfite.
Preferably, drying temperature is 60 ~ 70 DEG C.
The invention provides two kinds of preparation types：Oral liquid and pulvis, preparation method are respectively：
The preparation method of oral liquid：The g of 100 mL oral liquids aluminium complex containing baicalein 1 ~ 5, preparation process are：
Baicalein aluminium complex is dissolved in cosolvent, heating is stirred continuously, and it is complete to solution that alkali lye regulation pH value is added dropwise
Clarification, formula ratio is complemented to water, is finally adjusted back pH to 6 ~ 7 with hydrochloric acid solution, is produced oral liquid；Wherein, the cosolvent is
The one or more of combination therein of dimethylformamide, glycerine, absolute ethyl alcohol, PEG 200, dimethyl sulfoxide (DMSO).
Preferably, in terms of mass volume ratio g/mL, dimethylformamide, glycerine, absolute ethyl alcohol, PEG 200, dimethyl
When sulfoxide is as cosolvent, the amount ratio with baicalein aluminium complex is respectively：Baicalein aluminium complex: dimethylformamide=1
∶5~10；Baicalein aluminium complex: glycerine=1: 8 ~ 10；Baicalein aluminium complex: absolute ethyl alcohol=1: 5 ~ 8；Baicalein aluminium is complexed
Thing: PEG 200=1: 6 ~ 10；Baicalein aluminium complex: dimethyl sulfoxide (DMSO)=1: 5 ~ 8.
Preferably, heating-up temperature is 50 ~ 70 DEG C.
The preparation method of pulvis：The g of 100 g pulvises aluminium complex containing baicalein 1 ~ 5, preparation process are：
Baicalein aluminium complex is dissolved by heating in PEG6000, after cooling crush, adds sodium acid carbonate and pharmaceutical carrier mixing
Uniformly, pulvis is produced；Wherein, the pharmaceutical carrier is that lactose, oral glucose, sucrose, mannitol are therein one or more of
Combination.
Preferably, by quality ratio, baicalein aluminium complex and PEG6000 amount ratio are 1: 8 ~ 12, baicalein aluminium network
The ratio of compound and sodium acid carbonate is 1: 2.5 ~ 4, and pharmaceutical carrier complements to formula ratio.
The above-mentioned formulation of the present invention is mainly used in veterinary art, poultry：Be mainly used in the enteritis as caused by bacterium or virus,
Have loose bowels, the intestines problem such as punishment in advance and intestines poison syndrome；Pig：It is true to be mainly used in piglet Huang, dysentery characterized by white mucous stool, curative effect as caused by Escherichia coli
Cut.Usage：1. oral liquid：The kg of 100 mL oral liquids 50 ~ 100, mix drink or tank clothes；2. pulvis：100 g pulvises mix full price
The kg of feed 25 ~ 50, free choice feeding.
Beneficial effect：Formulation of the present invention is mainly used in veterinary art, to develop the animal drugs of new type of safe green noresidue
Product provide new direction.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described.It should be understood that following examples are merely to illustrate this
Invention is not for limitation the scope of the present invention.
Embodiment 1
A kind of preparation method of baicalein aluminium complex：Take the g of baicalein 20 to add in 600 mL distilled water, 2 are added dropwise while stirring
Mol/L NaOH solution, it is 6.7 to solution ph, now solution is clarified；Saturation liquor alumini chloridi is added dropwise while stirring, originally
Brick-red flocculent deposit is produced, until stopping addition when no longer producing floccule；Stand overnight, supernatant discarding, and it is sub- with 0.2%
Sodium bisulphate solution after washing precipitate 3 times, 60 DEG C of dryings, produces baicalein aluminium complex repeatedly.
Embodiment 2
A kind of preparation method of baicalein aluminium complex：Take the g of baicalein 300 to add in 1000 mL distilled water, drip while stirring
Add 2 mol/L NaHCO3Solution, it is 6.8 to solution ph, now solution is clarified；It is molten that saturated acetic acid aluminium is added dropwise while stirring
Liquid, orange red flocculent deposit is originally produced, until stopping addition when no longer producing floccule；Stand overnight, supernatant discarding, be used in combination
0.2% aqueous solution of sodium bisulfite after washing precipitate 3 times, 60 DEG C of dryings, produces baicalein aluminium complex repeatedly.
Embodiment 3-- oral liquids
The preparation method of oral liquid：Example 1 prepare the g of baicalein aluminium complex 3, add 18 mL dimethylformamides and
The mL of glycerine 24,60 DEG C of insulations, the NaOH solution side edged for instilling 2 mol/L quickly stir, are clarified to solution, use distilled water
100 mL are settled to, then it is 6.5 to adjust pH value with 2 mol/L HCL.
Embodiment 4-- pulvises
The preparation method of pulvis：The g of PEG6000 30 are taken, baicalein aluminium complexing prepared by embodiment 2 is added after melting in 60 DEG C
Thing 3 g, it is stirring while adding complete to the dissolving of baicalein aluminium complex, crushed after putting 4 DEG C of coolings rapidly, add 9 g bicarbonates
Sodium, mannitol are supplemented to 100 g.
Clinical effectiveness
Effect example 1
Yingyang Mr. Wang raises a sow, is farrowed 12 in 2 months 2016, and symptom of diarrhea occurs in 5 days postpartum, full nest piglet,
Affected pig lassitude, slightly disorderly, most of piglet row white is dirty smelly, carries trace of blood excrement secretly for hair.Therapeutic scheme：By 3 mouthfuls of embodiment
Take the mL of liquid 100 and be watered 100 kg, every piglet tank takes 5 mL, and once a day, continuous tank takes 3d, and piglet returns to normal, 5d
Clinical symptoms all disappear afterwards, and the later stage does not recur.
Effect example 2
The feed lot of Xinzheng one, white meat-type chickens 8000 are raised, because weather turns cold, mismanagement, burst spirit is not during 32 age in days
Shake, feed intake declines, and has loose bowels, punishment in advance, through cut open inspection, finds intestinal mucosa swelling, bleeding, partial exfoliation.Therapeutic scheme：100 mL
The oral liquid of embodiment 3 is watered 100 kg, free water, and excrement is molded after 4d, and excrement is normal after 5d, and clinical symptom disappearance, 7d
Feed intake substantially rises afterwards, does not occur similar symptom then, illustrates thorough treatment.
Claims (9)
- A kind of 1. preparation method of baicalein aluminium complex, it is characterised in that：Baicalein is added to the water, alkali is added dropwise while stirring Solution, it is 6.5 ~ 7 to solution ph；Saturation aluminum contained compound solution is added dropwise while stirring, until stopping when no longer producing floccule Only add；Stand overnight, supernatant discarding, and with after aqueous antioxidant solution repeatedly washing precipitate, dry, produce baicalein aluminium Complex compound.
- 2. the preparation method of baicalein aluminium complex as claimed in claim 1, it is characterised in that：The mass ratio of baicalein and water is 1∶30~40。
- 3. the preparation method of baicalein aluminium complex as claimed in claim 1, it is characterised in that：The aqueous slkali is 2 ~ 3 mol/ The NaHCO of L NaOH solution or 2 ~ 3 mol/L3Solution；The saturation aluminum contained compound solution is saturation liquor alumini chloridi, satisfied With aluminum hydroxide solution, saturation alumina solution, saturation aluminum sulfate solution or saturated acetic acid aluminum solutions；The antioxidant is water-soluble The mass concentration of liquid is 0.2 ~ 0.3 %, and the antioxidant is sodium hydrogensulfite, vitamin C or sodium pyrosulfite.
- 4. the preparation method of baicalein aluminium complex as claimed in claim 1, it is characterised in that：Drying temperature is 60 ~ 70 DEG C.
- 5. one kind prepares the side of oral liquid formulations using the baicalein aluminium complex as made from claim 1 ~ 4 any preparation method Method, it is characterised in that：The g of 100 mL oral liquids aluminium complex containing baicalein 1 ~ 5, preparation process are：Baicalein aluminium complex is dissolved in cosolvent, heating is stirred continuously, and it is complete to solution that alkali lye regulation pH value is added dropwise Clarification, formula ratio is complemented to water, is finally adjusted back pH to 6 ~ 7 with hydrochloric acid solution, is produced oral liquid；Wherein, the cosolvent is dimethylformamide, glycerine, absolute ethyl alcohol, PEG 200, dimethyl sulfoxide (DMSO) therein one Kind or several combinations.
- 6. the preparation method of oral liquid formulations as claimed in claim 5, it is characterised in that：In terms of mass volume ratio g/mL, diformazan When base formamide, glycerine, absolute ethyl alcohol, PEG 200, dimethyl sulfoxide (DMSO) are as cosolvent, the use with baicalein aluminium complex Measuring ratio is respectively：Baicalein aluminium complex: dimethylformamide=1: 5 ~ 10；Baicalein aluminium complex: glycerine=1: 8 ~ 10；Baicalein aluminium Complex compound: absolute ethyl alcohol=1: 5 ~ 8；Baicalein aluminium complex: PEG 200=1: 6 ~ 10；Baicalein aluminium complex: dimethyl sulfoxide (DMSO) =1∶5~8。
- 7. the preparation method of oral liquid formulations as claimed in claim 5, it is characterised in that：Heating-up temperature is 50 ~ 70 DEG C.
- 8. one kind prepares the side of pulvis preparation using the baicalein aluminium complex as made from claim 1 ~ 4 any preparation method Method, it is characterised in that：The g of 100 g pulvises aluminium complex containing baicalein 1 ~ 5, preparation process are：Baicalein aluminium complex is dissolved by heating in PEG6000, after cooling crush, adds sodium acid carbonate and pharmaceutical carrier mixing Uniformly, pulvis is produced；Wherein, the pharmaceutical carrier is lactose, oral glucose, sucrose, mannitol one or more of combination therein.
- 9. the preparation method of pulvis preparation described in claim 8, it is characterised in that：By quality ratio, baicalein aluminium complex Amount ratio with PEG6000 is 1: 8 ~ 12, and the ratio of baicalein aluminium complex and sodium acid carbonate is 1: 2.5 ~ 4, and pharmaceutical carrier is mended Enough to formula ratio.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111000896A (en) * | 2019-12-30 | 2020-04-14 | 武汉回盛生物科技股份有限公司 | Method for preparing baicalein metal complex by ore coagulation method and preparation thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105481916A (en) * | 2014-09-15 | 2016-04-13 | 闻永举 | Preparation method of flavone aglycone or monoglycoside from aluminum-salt-flavonoid-glycoside complex through hydrolysis |
-
2017
- 2017-10-18 CN CN201710971843.XA patent/CN107721962A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105481916A (en) * | 2014-09-15 | 2016-04-13 | 闻永举 | Preparation method of flavone aglycone or monoglycoside from aluminum-salt-flavonoid-glycoside complex through hydrolysis |
Non-Patent Citations (6)
| Title |
|---|
| 北京医学院革命委员会编: "《中草药制剂资料选编》", 31 December 1971, 北京医学院 * |
| 周学文等: "克痢沙防治猪鸡细菌性泻痢试验研究", 《云南畜牧兽医》 * |
| 崔耀明主编: "《兽药制剂工艺》", 31 August 2007, 中国农业大学出版社 * |
| 杨海峰主编: "《动物医药专业技能实训教程》", 30 September 2010, 中国轻工业出版社 * |
| 蒋建军: "高纯黄芩素的制备及化学修饰", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
| 贾林军等主编: "《动物药理学》", 31 January 2017, 中国轻工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111000896A (en) * | 2019-12-30 | 2020-04-14 | 武汉回盛生物科技股份有限公司 | Method for preparing baicalein metal complex by ore coagulation method and preparation thereof |
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Application publication date: 20180223 |