CN101991547A - Preparation method of sodium ferulate freeze-dried powder injection - Google Patents
Preparation method of sodium ferulate freeze-dried powder injection Download PDFInfo
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- CN101991547A CN101991547A CN2009100752445A CN200910075244A CN101991547A CN 101991547 A CN101991547 A CN 101991547A CN 2009100752445 A CN2009100752445 A CN 2009100752445A CN 200910075244 A CN200910075244 A CN 200910075244A CN 101991547 A CN101991547 A CN 101991547A
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Abstract
The invention discloses a preparation method of a sodium ferulate freeze-dried powder injection, comprising the following steps of: (a) firstly, adding water for injection, with the volume being about 80 percent of the pre-compounding volume, into a compounding tank, controlling the water temperature at 15-20 DEG C, adding raw sodium ferulate powder, detecting a pH value, and enabling the pH value to be between 6.8 and 7.2; adding activated carbon, replenishing water to reach a certain volume, stirring, decoloring, removing pyrogen, filtering, detecting the content and split charging; and (b), carrying out freeze drying according to the following steps of, firstly, pre-freezing: placing a product on a clapboard of a freeze drying box, cooling the product to 40-45 DEG C below zero, keeping the temperature for 4-6h; secondly, sublimating: heating the product to 4-6 DEG C below zero, keeping the temperature for 1h, cooling to 40-45 DEG C below zero, and keeping the temperature for 2-3h; and thirdly, separating out and drying. A technical formula of the method does not contain any excipient or other adjuncts and only contains ferulic acid sodium. The prepared preparation has loose texture, good resolubility and strong stability.
Description
Technical field:
The present invention relates to the preparation method of medicine, specifically to the preparation method of the sodium ferulate freeze dried powder injection of saying so.
Background technology
Sodium ferulate is non-peptide-like endothelin receptor antagonist, but the vasoconstriction that the antagonism Endothelin causes, boosts and vascular smooth muscle cell proliferation, alleviates vascular endothelial injury; Increase the synthetic of NO, lax vascular smooth muscle; Anticoagulant, anticoagulation, improve the hemorheology feature.This product also can suppress the synthetic of cholesterol, and blood fat reducing is removed free radical, the control lipid peroxidation injury; The enhance immunity function, and certain analgesia, spasmolysis are arranged.
When the preparation sodium ferulate freeze dried powder injection, to add the quality that improves its dissolubility and product than strong dose with adjuvant usually at present.As the preparation method of the disclosed a kind of sodium ferulate freeze dried powder injection of CN1830427, be exactly with sodium ferulate after hyperfiltration technique is handled, with mannitol filtrate in lucifuge, feed under the condition of nitrogen gas and prepare, fill forms through after the lyophilization.Yet amount of excipient is too much, is not only the cost that increases product, and main is to introduce unnecessary impurity in product, and then influences patient's drug safety.CN1561981 also discloses a kind of preparation method of sodium ferulate freeze dried powder injection, this method is that the sodium ferulate crude drug is dissolved in the sterile water for injection, stir, filter, to send into freezer dryer in the bottle of packing into filtrate branch, under-20 ℃ of conditions, 30～40 minutes evacuation is carried out in 2～3 hours quick-freezing again, carries out subliming by heating, parsing-desiccation then.This method prepares sodium ferulate freeze dried powder injection, and its outward appearance subsides, it is poor to freeze type, and solubility and clarity are wayward.
Summary of the invention
Purpose of the present invention just provides the preparation method that a kind of preparation does not contain excipient, stability is high, solubility is good and outward appearance is full sodium ferulate dry powder injection.
The object of the present invention is achieved like this:
The preparation method of sodium ferulate freeze dried powder injection provided by the present invention, it may further comprise the steps:
(a) water for injection of the about 80% prewired volume of adding in material-compound tank is controlled at 15～20 ℃ with water temperature, adds the former powder of sodium ferulate, detects pH value, makes them between 6.8～7.2; Add active carbon, supply volume with residue water for injection, stirring is decoloured, desuperheating is former, filters detection level, packing;
(b) according to the following steps lyophilizing:
(1) pre-freeze: goods are placed on the freeze drying box dividing plate, make goods be chilled to-40～-45 ℃, be incubated 4～6 hours;
(2) distillation: goods are warming up to-4～-6 ℃ of insulations 1 hour, reduce to-40～-45 ℃ again, be incubated 2～3 hours; And condenser is cooled to below-45 ℃, evacuation, control vacuum is at 10～20pa;
(3) parsing-desiccation: heat up 5 ℃ with per 1.5 hours, be about-30 ℃ to products temperature, after this slowly heating up rises to 20 ℃ with products temperature, is incubated 10 hours.
The inventive method does not contain any excipient or other adjuvants at the preparation sodium ferulate freeze dried powder injection in the technical recipe, only contain sodium ferulate.It is dissolved in the water for injection, under low temperature, lucifuge, feeding condition of nitrogen gas, prepares, fill, through the lyophilization of special process design, made preparation quality is loose, solubility is good, stability is strong again.
Sodium ferulate freeze dried powder injection provided by the invention, its clinical indication is identical with common injection of sodium ferulate.
Usage and consumption can references: intravenous drip.A 0.1～0.3g, 1 time on the one, dissolving back adds quiet of glucose injection, normal saline or Dextrose and Sodium Chloride Inj. 100～500ml.Intramuscular injection.A 0.1g 1～2 time on the one, faces with preceding and dissolves with normal saline 2～4ml.Be 10 days a course of treatment.
The specific embodiment:
Further specify the present invention below in conjunction with specific embodiment.
Embodiment 1
Every 2ml water for injection of sodium ferulate freeze dried powder injection 0.15g sodium ferulate.
Preparation process:
A, in material-compound tank, add the water for injection of about 80% prewired volume, water temperature is controlled at 20 ℃, the lucifuge operation.Pour nitrogen in material-compound tank, add the former powder of sodium ferulate of recipe quantity, the limit edged stirs, and makes its dissolving, detects pH value in this process, makes them between 6.8～7.2.The needle-use activated carbon of 0.1% (g/ml) is added in the above-mentioned solution, supply volume with residue water for injection.Stir and add filter paper by filter press after 30 minutes and take off charcoal.Laboratory sampling detects pH value, carries out aseptic filter pressing after qualified.Filter at hundred grades of indoor microporous filter membrane filters that pass through 0.22 μ m of clean packing, carry out liquid medicine filling according to the medicinal liquid loading amount, and carry out automatic false add plug, on the freeze drying box internal partition of semi-finished product being put into cleaning then, shut chamber door, lyophilization is carried out to medicinal liquid in the lyophilizing post.
Refrigerating process:
(1) pre-freeze: the medicine that branch is installed places on the freeze drying box dividing plate, makes goods be chilled to-40 ℃, is incubated 4 hours.
(2) distillation: goods are warming up to-4 ℃ of insulations 2 hours, reduce to-40 ℃ of insulations 2 hours again.And condenser is cooled to below-45 ℃, evacuation, control vacuum is at 10～20pa.
(3) parsing-desiccation: heat up 5 ℃ with per 1.5 hours, with plate temperature rise to 0 ℃, this moment, products temperature was about-30 ℃, and after this slowly heating up rises to 20 ℃ with products temperature.This process is about 24 hours.20 ℃ of insulations 10 hours.
After treating that above-mentioned steps is finished, outlet.Roll lid, lamp inspection, packing.
Prepare three batches of products according to the method described above, 5000 every batch, stipulate down to detect result's following (seeing Table 1) according to 2000 editions Chinese Pharmacopoeia medicine items.
Table 1
By detecting data as can be known: this technology preparation is more stable, and every quality index is qualified, stable.
Embodiment 2
(a) water for injection of the about 80% prewired volume of adding in material-compound tank is controlled at 15 ℃ with water temperature, adds the former powder of sodium ferulate, detects pH value, makes it 6.8; Add 0.2% (g/ml) active carbon, supply volume with residue water for injection, stirring is decoloured, desuperheating is former, filters detection level, packing;
(b) according to the following steps lyophilizing:
(1) pre-freeze: goods are placed on the freeze drying box dividing plate, make goods be chilled to-45 ℃, be incubated 6 hours;
(2) distillation: goods are warming up to-6 ℃ of insulations 2 hours, reduce to-40～45 ℃ again, and condenser is cooled to below-45 ℃, evacuation, control vacuum is incubated 3 hours at 10～20pa;
(3) parsing-desiccation: heat up 5 ℃ with per 1.5 hours, be about-30 ℃ to products temperature, after this slowly heating up rises to 20 ℃ with products temperature, is incubated 8 hours.
Its product quality testing result of embodiment 2 products made therebies is substantially the same manner as Example 1.
Reference examples 1
Get aseptic sodium ferulate crude drug 5kg, be dissolved among the sterile water for injection 100kg, stir filtration in 15 minutes, after sending into freezer dryer in the clean cillin bottle of packing into filtrate branch.Carry out-20 ℃, 2～3 hours quick-freezing, the evacuation that carried out again 30～40 minutes makes water vapor pressure between the 450-500 handkerchief, then products temperature is risen to-25 ℃, is incubated 30～38 hours, is warming up to 40 ℃ then.When products temperature reached 40 ℃, insulation top plug, was rolled lid more than 2 hours.
Preparing three batches of products (5000 every crowd of 090401s, 090402s, 090403s) in this way contrasts with embodiment 1 made three batches of products (090401,090402,090403).
Result of the test sees table 2 for details
The method of testing of solubility wherein: at normal temperatures, every lyophilized formulations adds the time when meter dissolves fully behind the 2ml water for injection.
This shows that its quality of sodium ferulate freeze dried powder injection provided by the invention obviously is better than prior art.
Claims (2)
1. the preparation method of a sodium ferulate freeze dried powder injection is characterized in that it may further comprise the steps:
(a) water for injection of the about 80% prewired volume of adding in material-compound tank is controlled at 15～20 ℃ with water temperature, adds the former powder of sodium ferulate, detects pH value, makes them between 6.8～7.2; Add active carbon, supply volume with residue water for injection, stirring is decoloured, desuperheating is former, filters detection level, packing;
(b) according to the following steps lyophilizing:
(1) pre-freeze: goods are placed on the freeze drying box dividing plate, make goods be chilled to-40～-45 ℃, be incubated 4～6 hours;
(2) distillation: goods are warming up to-4～-6 ℃ of insulations 1 hour, reduce to-40～45 ℃ again, and condenser is cooled to below-45 ℃, evacuation, control vacuum is incubated 2～3 hours at 10～20pa;
(3) parsing-desiccation: heat up 5 ℃ with per 1.5 hours, be about-30 ℃ to products temperature, after this slowly heating up rises to 20 ℃ with products temperature, is incubated 8～10 hours.
2. according to the preparation method of the described sodium ferulate freeze dried powder injection of claim 1, it is characterized in that in process for preparation, pouring nitrogen protection.
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| CN2009100752445A CN101991547A (en) | 2009-08-21 | 2009-08-21 | Preparation method of sodium ferulate freeze-dried powder injection |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111773187A (en) * | 2020-06-15 | 2020-10-16 | 北京和舆医药科技有限公司 | Dexamethasone sodium phosphate freeze-dried powder injection |
| CN112472674A (en) * | 2021-01-06 | 2021-03-12 | 福安药业集团湖北人民制药有限公司 | Preparation method of sodium ferulate freeze-dried powder injection |
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2009
- 2009-08-21 CN CN2009100752445A patent/CN101991547A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111773187A (en) * | 2020-06-15 | 2020-10-16 | 北京和舆医药科技有限公司 | Dexamethasone sodium phosphate freeze-dried powder injection |
| CN112516091A (en) * | 2020-06-15 | 2021-03-19 | 和舆(苏州)医药科技有限公司 | Dexamethasone sodium phosphate freeze-dried powder injection |
| CN112516091B (en) * | 2020-06-15 | 2022-03-29 | 和舆(苏州)医药科技有限公司 | Dexamethasone sodium phosphate freeze-dried powder injection |
| CN111773187B (en) * | 2020-06-15 | 2022-08-19 | 和舆(苏州)医药科技有限公司 | Dexamethasone sodium phosphate freeze-dried powder injection |
| CN112472674A (en) * | 2021-01-06 | 2021-03-12 | 福安药业集团湖北人民制药有限公司 | Preparation method of sodium ferulate freeze-dried powder injection |
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Application publication date: 20110330 |