CN106474078A - The preparation method of Andrographolide in Andrographolide for Injection - Google Patents
The preparation method of Andrographolide in Andrographolide for Injection Download PDFInfo
- Publication number
- CN106474078A CN106474078A CN201510857567.5A CN201510857567A CN106474078A CN 106474078 A CN106474078 A CN 106474078A CN 201510857567 A CN201510857567 A CN 201510857567A CN 106474078 A CN106474078 A CN 106474078A
- Authority
- CN
- China
- Prior art keywords
- andrographolide
- injection
- preparation
- microporous membrane
- coarse filtration
- 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.)
- Pending
Links
Classifications
-
- 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
- A61K9/19—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles lyophilised, i.e. freeze-dried, solutions or dispersions
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
- A61K31/365—Lactones
-
- 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
- A61K47/02—Inorganic compounds
-
- 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
- A61K9/0012—Galenical forms characterised by the site of application
- A61K9/0019—Injectable compositions; Intramuscular, intravenous, arterial, subcutaneous administration; Compositions to be administered through the skin in an invasive manner
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Veterinary Medicine (AREA)
- Medicinal Chemistry (AREA)
- Dermatology (AREA)
- Engineering & Computer Science (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Inorganic Chemistry (AREA)
- Medicinal Preparation (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention belongs to a kind of pharmaceutical technology field, it is specifically related to a kind of preparation method of Andrographolide in Andrographolide for Injection, step is：（1）, andrographolide is added in water for injection, stirring is so as to abundant dissolve；It is subsequently adding sodium-chloride water solution, stirs, holding pH is 6.5-7.5, obtains andrographolide solution；（2）, activated carbon is added to above-mentioned andrographolide solution, stir, with microporous membrane cylindrical filter cartridge filter coarse filtration, obtain coarse filtration liquid；（3）, by above-mentioned coarse filtration liquid and water for injection mixing, stir, with 0.2 μm of microporous membrane cylindrical filter cartridge filter aseptic filtration, lyophilizing, obtain Andrographolide in Andrographolide for Injection；The good stability of Andrographolide in Andrographolide for Injection liquid of the present invention, impurity content is low, has no adverse reaction, very big improve the efficiency of product it is ensured that the purity of medicinal liquid, improve drug safety.
Description
Technical field
The invention belongs to a kind of pharmaceutical technology field, it is specifically related to a kind of preparation method of Andrographolide in Andrographolide for Injection.
Background technology
Andrographolide is the new derivatives of Chinese medicine Herba Andrographis extract andrographolide, chemical name is 14- deshydroxy -11,12- bis- dehydrogenation andrographolide -3,19- disuccinic acid half ester k-na salt monohydrate, the preparation of this product is presently mainly liquid drugs injection or freeze-dried powder, early stage capillary permeability clinically can be suppressed to increase and inflammatory exudation and edema, can specifically excited Pituitary Adrenalcortical function, promote adrenocortical hormone（ACTH）Release, increases the biosynthesiss of ACTH in antepituitary；There is the effect of multiple virus such as inactivated adenovirus, influenza virus, Respiroviruses in vitro.It is primarily adapted for use in viral pneumonia and viral upper respiratory tract infection, be one of more conventional medicine in current tcm emergency.
Andrographolide is readily soluble in water, in ethanol slightly soluble, insoluble in acetone or ether.
The patent application of Chinese Patent Application No. 201210595056.7 discloses a kind of ' Tanhuning ' injection and preparation method thereof, it is made up of citric acid than 0.1～0.5% of the Cysteine Hydrochloride than 0.1～0.5% for the weight, weight, volume ratio 2.5～7.5% propylene glycol, andrographolide and water for injection, the content of andrographolide is every ml injection 5～40mg.Comprise the steps：
1. weigh Cysteine Hydrochloride, citric acid, put in sterile chamber, add the water for injection of full dose 70%, stirring and dissolving；
2. measure propylene glycol add step 1. in, after stirring and evenly mixing, adjust pH value to 6.5-7.5 with the sodium hydroxide solution of 1mol/L；
3. weigh andrographolide, be added to step 2. in, after stirring and dissolving, water for injection constant volume；
4. add the medicinal charcoal of 0.05%w/v, stirring and adsorbing 15-30min, microporous filter membrane coarse filtration, de- charcoal, filtration, detection, fine straining, nitrogen charging in step solution 3., roll lid, sterilizing, thus obtaining the product ' Tanhuning ' injection.
Content of the invention
The technical problem to be solved in the present invention is to provide that a kind of impurity content is low, the preparation method of good stability Andrographolide in Andrographolide for Injection.
The present invention is a kind of preparation method of Andrographolide in Andrographolide for Injection, and step is：
（1）, andrographolide is added in water for injection, stirring is so as to abundant dissolve；It is subsequently adding sodium-chloride water solution, stirs, holding pH is 6.5-7.5, obtains andrographolide solution；
（2）, activated carbon is added to above-mentioned andrographolide solution, stir, with microporous membrane cylindrical filter cartridge filter coarse filtration, obtain coarse filtration liquid；
（3）, by above-mentioned coarse filtration liquid and water for injection mixing, stir, with 0.2 μm of microporous membrane cylindrical filter cartridge filter aseptic filtration, lyophilizing, obtain Andrographolide in Andrographolide for Injection.
Preferably, described step（2）In the microporous membrane cylindrical filter cartridge filter used be 0.65 μm -0.45 μm microporous membrane cylindrical filter cartridge filter.
Described step（1）PH be preferably 7.
In described 100ml Andrographolide in Andrographolide for Injection, the content of each component is：Andrographolide 60-70mg, sodium chloride 1-1.5g, activated carbon 1-2g.
Described step of freeze drying is, by the product after filtering between -45 DEG C -35 DEG C pre-freeze 1-4 hour, be then cooled to -60 DEG C of holding 1-3 hours, control vacuum in below 20MPa, be to slowly warm up to -25 DEG C, the heating-up time is 10h, continue to be to slowly warm up to 5 DEG C, the heating-up time is 8-10h；It is continuously heating to 25 DEG C, the heating-up time is 1-3h, in 25 DEG C of heat preservation and dryness 1-3h, obtains Andrographolide in Andrographolide for Injection.
The invention has the beneficial effects as follows, the good stability of Andrographolide in Andrographolide for Injection liquid of the present invention, impurity content is low, has no adverse reaction, very big improve the efficiency of product it is ensured that the purity of medicinal liquid, improve drug safety.
Specific embodiment
Embodiment 1
The step of the preparation method of Andrographolide in Andrographolide for Injection of the present invention is：
（1）, andrographolide is added in water for injection, stirring is so as to abundant dissolve；It is subsequently adding sodium-chloride water solution, stirs, keep pH to be 7, obtain andrographolide solution；
（2）, activated carbon is added to above-mentioned andrographolide solution, stir, with 0.65 μm, 0.45 μm of microporous membrane cylindrical filter cartridge filter coarse filtration respectively, obtain coarse filtration liquid；
（3）, by above-mentioned coarse filtration liquid and water for injection mixing, stir, with 0.2 μm of microporous membrane cylindrical filter cartridge filter aseptic filtration, lyophilizing, obtain Andrographolide in Andrographolide for Injection.
In described 100ml Andrographolide in Andrographolide for Injection, the content of each component is：Andrographolide 60mg, sodium chloride 1g, activated carbon 2g.
Described step of freeze drying is, by the product after filtering between -40 DEG C pre-freeze 4 hours, be then cooled to -60 DEG C and keep 1 hour, control vacuum in below 20MPa, be to slowly warm up to -25 DEG C, the heating-up time is 10h, continues to be to slowly warm up to 5 DEG C, the heating-up time is 8h；It is continuously heating to 25 DEG C, the heating-up time is 1h, in 25 DEG C of heat preservation and dryness 3h, obtains Andrographolide in Andrographolide for Injection.
The Andrographolide in Andrographolide for Injection that embodiment 1 is prepared is detected, its LC total impurities is 0.8%, and in the case of 40 DEG C of high temperature storage 30 days, impurity content does not substantially rise.
Embodiment 2
（1）, andrographolide is added in water for injection, stirring is so as to abundant dissolve；It is subsequently adding sodium-chloride water solution, stirs, keep pH to be 6.5, obtain andrographolide solution；
（2）, activated carbon is added to above-mentioned andrographolide solution, stir, with 0.65 μm, 0.45 μm of microporous membrane cylindrical filter cartridge filter coarse filtration respectively, obtain coarse filtration liquid；
（3）, by above-mentioned coarse filtration liquid and water for injection mixing, stir, with 0.2 μm of microporous membrane cylindrical filter cartridge filter aseptic filtration, lyophilizing, obtain Andrographolide in Andrographolide for Injection.
In described 100ml Andrographolide in Andrographolide for Injection, the content of each component is：Andrographolide 70mg, sodium chloride 1.5g, activated carbon 1g.
Described step of freeze drying is, by the product after filtering between -45 DEG C pre-freeze 1 hour, be then cooled to -60 DEG C and keep 3 hours, control vacuum in below 20MPa, be to slowly warm up to -25 DEG C, the heating-up time is 10h, continues to be to slowly warm up to 5 DEG C, the heating-up time is 10h；It is continuously heating to 25 DEG C, the heating-up time is 3h, in 25 DEG C of heat preservation and dryness 1h, obtains Andrographolide in Andrographolide for Injection.
The Andrographolide in Andrographolide for Injection that embodiment 1 is prepared is detected, its LC total impurities is 0.9%, and in the case of 40 DEG C of high temperature storage 30 days, impurity content does not substantially rise.
Claims (5)
1. a kind of preparation method of Andrographolide in Andrographolide for Injection, is characterized in that, step is：
（1）, andrographolide is added in water for injection, stirring is so as to abundant dissolve；It is subsequently adding sodium-chloride water solution, stirs, holding pH is 6.5-7.5, obtains andrographolide solution；
（2）, activated carbon is added to above-mentioned andrographolide solution, stir, with microporous membrane cylindrical filter cartridge filter coarse filtration, obtain coarse filtration liquid；
（3）, by above-mentioned coarse filtration liquid and water for injection mixing, stir, with 0.2 μm of microporous membrane cylindrical filter cartridge filter aseptic filtration, lyophilizing, obtain Andrographolide in Andrographolide for Injection.
2. the preparation method of Andrographolide in Andrographolide for Injection as claimed in claim 1, is characterized in that, described step（2）In the microporous membrane cylindrical filter cartridge filter used be 0.65 μm -0.45 μm microporous membrane cylindrical filter cartridge filter.
3. the preparation method of Andrographolide in Andrographolide for Injection as claimed in claim 1, is characterized in that, described step（1）PH be 7.
4. the preparation method of Andrographolide in Andrographolide for Injection as claimed in claim 1 or 2, is characterized in that, in described 100ml Andrographolide in Andrographolide for Injection, the content of each component is：Andrographolide 60-70mg, sodium chloride 1-1.5g, activated carbon 1-2g.
5. the preparation method of Andrographolide in Andrographolide for Injection as claimed in claim 1 or 2, it is characterized in that, described step of freeze drying is, by filter after product between -45 DEG C -35 DEG C pre-freeze 1-4 hour, be then cooled to -60 DEG C holding 1-3 hours, control vacuum in below 20MPa, it is to slowly warm up to -25 DEG C, heating-up time is 10h, continues to be to slowly warm up to 5 DEG C, and the heating-up time is 8-10h；It is continuously heating to 25 DEG C, the heating-up time is 1-3h, in 25 DEG C of heat preservation and dryness 1-3h, obtains Andrographolide in Andrographolide for Injection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510857567.5A CN106474078A (en) | 2015-11-30 | 2015-11-30 | The preparation method of Andrographolide in Andrographolide for Injection |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510857567.5A CN106474078A (en) | 2015-11-30 | 2015-11-30 | The preparation method of Andrographolide in Andrographolide for Injection |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106474078A true CN106474078A (en) | 2017-03-08 |
Family
ID=58238480
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510857567.5A Pending CN106474078A (en) | 2015-11-30 | 2015-11-30 | The preparation method of Andrographolide in Andrographolide for Injection |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106474078A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107281143A (en) * | 2017-07-27 | 2017-10-24 | 哈尔滨松鹤制药有限公司 | A kind of Andrographolide in Andrographolide for Injection freeze drying powder injection and preparation method thereof |
| CN110467589A (en) * | 2019-08-28 | 2019-11-19 | 武汉大学 | A kind of preparation method of andrographolide sterile bulk drug |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101270101A (en) * | 2008-05-08 | 2008-09-24 | 海南斯达制药有限公司 | Method for preparing potassium sodium dehydroandroan drographolide succinate for injection and its freeze-dried injection |
| CN101780051A (en) * | 2008-05-08 | 2010-07-21 | 海南斯达制药有限公司 | Preparation methods of potassium sodium dehydroandroan drographolide succinate and freeze-dried powder injection thereof |
| CN102885775A (en) * | 2011-07-19 | 2013-01-23 | 重庆莱美药业股份有限公司 | Andrographolide sterile powder and its preparation method |
| CN103494779A (en) * | 2013-09-30 | 2014-01-08 | 悦康药业集团有限公司 | Andrographolide powder preparation for injection and preparation method thereof |
-
2015
- 2015-11-30 CN CN201510857567.5A patent/CN106474078A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101270101A (en) * | 2008-05-08 | 2008-09-24 | 海南斯达制药有限公司 | Method for preparing potassium sodium dehydroandroan drographolide succinate for injection and its freeze-dried injection |
| CN101780051A (en) * | 2008-05-08 | 2010-07-21 | 海南斯达制药有限公司 | Preparation methods of potassium sodium dehydroandroan drographolide succinate and freeze-dried powder injection thereof |
| CN102885775A (en) * | 2011-07-19 | 2013-01-23 | 重庆莱美药业股份有限公司 | Andrographolide sterile powder and its preparation method |
| CN103494779A (en) * | 2013-09-30 | 2014-01-08 | 悦康药业集团有限公司 | Andrographolide powder preparation for injection and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107281143A (en) * | 2017-07-27 | 2017-10-24 | 哈尔滨松鹤制药有限公司 | A kind of Andrographolide in Andrographolide for Injection freeze drying powder injection and preparation method thereof |
| CN110467589A (en) * | 2019-08-28 | 2019-11-19 | 武汉大学 | A kind of preparation method of andrographolide sterile bulk drug |
| CN110467589B (en) * | 2019-08-28 | 2023-04-07 | 武汉大学 | Preparation method of potassium sodium dehydroandroan drographolide succinate sterile bulk drug |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103209966A (en) | Sodium salt of 6-fluoro-3-hydroxy-2-pyrazine carboxamide | |
| CN102382082B (en) | Novel potassium sodium dehydroandroan drographolide succinate compound and drug combination thereof | |
| CN104435226A (en) | Paederia scandens extract and application thereof | |
| CN105078905A (en) | Preparation method of doxycycline hyclate freeze-dried powder injection | |
| CN106474078A (en) | The preparation method of Andrographolide in Andrographolide for Injection | |
| CN103864683B (en) | Medicine eutectic of ciprofloxacin and salicylic acid and preparation process thereof | |
| CN106389353A (en) | Compound ammonium glycyrrhetate S for injection, and preparation method therefor | |
| CN102614136B (en) | Potassium sodium dehydroandrographolide succinate composition for injection, and freeze-dried powder injection and preparation method for freeze-dried powder injection | |
| CN101148441A (en) | Andrographolidi natrii bisulfis and preparation method thereof | |
| CN104013585A (en) | Piracetam freeze-dried powder injection for injection and preparation method thereof | |
| CN104688676A (en) | Andrographolide concentrated liquid and medical application thereof | |
| WO2015024217A1 (en) | Chlorogenic acid powder-injection and preparation method thereof | |
| CN1947749B (en) | Medicine composition containing Poria cocos and Touhualiao (polygonaceae) | |
| CN104587452A (en) | Solution for preparing thymalfasin preparation and method for preparing thymalfasin preparation by virtue of solution | |
| CN103058999A (en) | Novel pantoprazole sodium compound and pharmaceutical composition thereof | |
| TW201417825A (en) | Compositions comprising antifungal drug and lactate buffer agent | |
| CN102940623B (en) | Medicinal composition of levocarnitine compound | |
| CN101491495A (en) | Salvianolic acid B magnesium injection, preparation method and use thereof | |
| CN106420711A (en) | Andrographolide composition, injection preparation of andrographolide composition and preparation method | |
| CN103739576A (en) | Novel antiviral andrographolide derivative and preparation method and application thereof | |
| CN102757471A (en) | Novel active cytidine disodium triphosphate compound and pharmaceutical composition thereof | |
| CN103751792A (en) | Application of angelica sinensis extract as natural intestinal absorption enhancer | |
| TW201907938A (en) | A use of an extract of Asplenium australasicum (J. Sm.) Hook | |
| CN108992394A (en) | A kind of preparation method of pseudoephedrine hydrochloride slow release preparation | |
| CN102895223A (en) | Dehydroandrographolide succinate compound-containing medicinal composition and its preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170308 |
|
| RJ01 | Rejection of invention patent application after publication |