CN104771367A - Preparation process of azlocillin sodium for injection - Google Patents
Preparation process of azlocillin sodium for injection Download PDFInfo
- Publication number
- CN104771367A CN104771367A CN201510200598.3A CN201510200598A CN104771367A CN 104771367 A CN104771367 A CN 104771367A CN 201510200598 A CN201510200598 A CN 201510200598A CN 104771367 A CN104771367 A CN 104771367A
- Authority
- CN
- China
- Prior art keywords
- azlocillin sodium
- azlocillin
- sodium
- preparation technology
- reagent bottle
- 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
Landscapes
- Medicinal Preparation (AREA)
- Medical Preparation Storing Or Oral Administration Devices (AREA)
Abstract
The invention relates to a preparation process of azlocillin sodium for injection. The preparation process comprises the following steps: synthesizing azlocillin sodium; and drying the synthesized azlocillin sodium, and preparing into powder, wherein the preparation process of the azlocillin sodium powder comprises the following steps: firstly, cleaning a reagent bottle for containing the azlocillin sodium powder, then quantitatively filling the azlocillin sodium powder into the cleaned reagent bottle according to a specification, filling nitrogen, then covering the bottle by using a pretreated rubber plug, then performing cover tying treatment by using an aluminum cover to ensure that the product is sealed, then sequentially performing inner label pasting, packaging and lamp inspection on the reagent bottle subjected to cover tying, then pasting an outer label on a packing box, and then performing inspection and packaging. The preparation process provided by the invention overcomes the problem that the existing preparation process of azlocillin sodium for injection reduces the medicinal effect of the azlocillin sodium for injection.
Description
Technical field
The present invention relates to medical drugs preparation technology field, particularly, relate to a kind of preparation technology of azlocillin sodium for injection.
Background technology
Azlocillin sodium, its chemical name is: (2S, 5R, 6R)-3,3-dimethyl-6-[(R)-2-(2-oxo-1-imidazolidine formamido group) this acetylamino of-2-]-7-oxo-4-thia-1-azabicyclo [3.2.0] heptane-2-formic acid sodium salt.
Azlocillin sodium by Bayer A.G take the lead in develop, in May, 1977 goes on the market, since twentieth century eighties, in state's application such as American and Britain, in nineteen eighty-three income American Pharmacopeia 20 editions ancillary volumes, 21 editions American Pharmacopeias in 1985 are appointed and are so recorded, it to the bactericidal action of bacillus pyocyaneus than Carbenicillin about large ten times, also there is the effect of the anti-Gram positive bacteria of ampicillin simultaneously, and retain the activity of Carbenicillin to intestinal bacteria, therefore from since the eighties in last century, extensive use has been obtained in countries such as American and Britain.China and in January, 1996 have issued New Drug Certificate and production licence to Zhejiang Zhejiang CONBA Pharmaceutical Co., Ltd, and have produced A Lexin injection powder injection by the said firm.
The effect and the safety that how to improve injecting drug use always are that pharmaceutical producing enterprise wishes the problem solved, the effect of injecting drug use solves from two aspects with safety is main, one is effect and the safety that Formulation guarantees medication, and two is effect and the safety that the process for producing of medicine guarantees medicine.Azlocillin sodium for injection is a most existing injection agent, and its prescription is single, guarantees that the effect of its medicine and safe main path are exactly by controlling its preparation technology.
The preparation technology of existing azlocillin sodium for injection causes the medicinal effects of azlocillin sodium for injection to reduce.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation technology of azlocillin sodium for injection, the problem of the medicinal effects reduction of the azlocillin sodium for injection caused with the preparation technology overcoming existing azlocillin sodium for injection.
The present invention's adopted technical scheme that solves the problem is: the preparation technology of azlocillin sodium for injection, comprises the following steps:
(1), the synthesis of azlocillin sodium: by dichloromethane and ampicillin by weight be that 1:0.064 ~ 1:0.068 mixes, regulate pH value of solution in alkalescence, obtain condensation reaction solution, under agitation put in above-mentioned condensation reaction solution by 1-Chlorocarbonyl-2-Imidazolidone with, dichloromethane, the weight ratio of 1-Chlorocarbonyl-2-Imidazolidone, dichloromethane and condensation reaction solution is 1:4.5:28 ~ 1:4.8:31; PH value of solution is regulated to be alkalescence, continue to stir, obtain condensation reaction material, water is adopted to carry out successively extract and separate to above-mentioned condensation reaction material, water layer is transferred in crystallizer, with acid for adjusting pH, crystalline solid centrifugal after crystallization, crystalline solid is washed and the azlocillin of drying, azlocillin is passed under the condition of cooling medium at retort interlayer and dissolves and the water in tank, after dissolving, add sodium hydroxide solution, add sodium bicarbonate solution and regulate pH, in solution, add depigmenting agent again, after filtration, sterilizing, obtain azlocillin sodium wet product;
(2), the azlocillin sodium wet product lyophilization of synthesis is prepared into Powdered by pulverizing and sieves;
(3), the preparation technology of azlocillin sodium: first cleaning is used for the reagent bottle of splendid attire azlocillin sodium powder, then azlocillin sodium powder is quantitatively loaded the above-mentioned reagent bottle cleaned by specification and be filled with nitrogen, then pretreated plug is covered, Zha Gai process is carried out again with aluminium lid, product is sealed, interior label, packaging, lamp inspection are pasted successively to the reagent bottle after Zha Gai, then labels outer on packing box, then test, pack.The medicinal effects of the azlocillin sodium for injection that the preparation technology of existing azlocillin sodium for injection causes reduces.Azlocillin sodium synthesis of the present invention completes in retort aseptic obtaining, the problem of what the introducing avoiding antibacterial caused the affect medicinal effects of azlocillin sodium, the present invention strictly carries out handle control to each operation in the preparation technology of azlocillin sodium, from wash bottle, subpackage, Zha Gai is to outer package, all sterilization treatment is carried out to working environment from use equipment, the problem that its result of use avoiding the performance impairment of the azlocillin sodium caused in son preparation process to cause reduces, so, the problem of the medicinal effects reduction of the azlocillin sodium for injection that the preparation technology that instant invention overcomes existing azlocillin sodium for injection causes.
Further, dichloromethane and ampicillin are 1:0.065 by weight.Dichloromethane and ampicillin are set to 1:0.065 by weight can make the two rapid solution.
Further, the weight ratio of 1-Chlorocarbonyl-2-Imidazolidone, dichloromethane and condensation reaction solution is 1:4.6:28.5.Improve the dissolved efficiency of 1-Chlorocarbonyl-2-Imidazolidone, dichloromethane and condensation reaction solution.
Further, the cleaning process of reagent bottle is followed successively by supersound washing, Shui Chong, air oven dry, oven for drying, sterilizing.Guarantee the thoroughly clean of reagent bottle and gnotobasis, avoid reagent bottle to have influence on the quality of azlocillin sodium.
Further, the plug of reagent bottle Zha Gai adopts rubber plug cleaning machine cleaning and sterilization treatment.Plug is avoided to have influence on the use of reagent bottle.
Further, aluminium lid need pass through and process, and pretreated concrete steps are: poured into by aluminium lid in clean porose stainless steel framework, add in electrically heated drying cabinet, be incubated powered-down after a hour.
To sum up, the invention has the beneficial effects as follows:
1, the present invention strictly carries out handle control to each operation in the preparation technology of azlocillin sodium, from wash bottle, subpackage, Zha Gai to outer package, all sterilization treatment is carried out to working environment, the problem that its result of use avoiding the performance impairment of the azlocillin sodium caused in preparation process to cause reduces from use equipment.
2, the present invention is 1:4.6:28.5 by dichloromethane and ampicillin being set to by weight the weight ratio of 1:0.065,1-Chlorocarbonyl-2-Imidazolidone, dichloromethane and condensation reaction solution; accelerate the mixing speed of solution, improve the efficiency of whole azlocillin sodium synthesis.
Detailed description of the invention
Below in conjunction with embodiment, to the detailed description further of invention do, but embodiments of the present invention are not limited thereto.
Embodiment:
The preparation technology of azlocillin sodium for injection, comprises the following steps:
(1), the synthesis of azlocillin sodium: dichloromethane and ampicillin are mixed by weight for 1:0.065, regulate pH value of solution in alkalescence, obtain condensation reaction solution, under agitation put in above-mentioned condensation reaction solution by 1-Chlorocarbonyl-2-Imidazolidone, dichloromethane, the weight ratio of 1-Chlorocarbonyl-2-Imidazolidone, dichloromethane and condensation reaction solution is 1:4.6:28.5; PH value of solution is regulated to be alkalescence, continue to stir, obtain condensation reaction material, water is adopted to carry out successively extract and separate to above-mentioned condensation reaction material, water layer is transferred in crystallizer, with acid for adjusting pH, crystalline solid centrifugal after crystallization, crystalline solid is washed and the azlocillin of drying, azlocillin is passed under the condition of cooling medium at retort interlayer and dissolves and the water in tank, after dissolving, add sodium hydroxide solution, add sodium bicarbonate solution and regulate pH, in solution, add depigmenting agent again, after filtration, sterilizing, obtain azlocillin sodium wet product;
(2), the azlocillin sodium wet product lyophilization of synthesis is prepared into Powdered by pulverizing and sieves;
(3), the preparation technology of azlocillin sodium: first cleaning is used for the reagent bottle of splendid attire azlocillin sodium powder, the cleaning process of reagent bottle is followed successively by supersound washing, water rushes, air is dried, oven for drying, sterilizing, then azlocillin sodium powder is quantitatively loaded the above-mentioned reagent bottle cleaned by specification and be filled with nitrogen, then pretreated plug is covered, Zha Gai process is carried out again with aluminium lid, product is sealed, successively interior label is pasted to the reagent bottle after Zha Gai, packaging, lamp inspection, then label outer on packing box, test again, packing, described plug adopts rubber plug cleaning machine cleaning and sterilization treatment, described aluminium lid need pass through and process, pretreated concrete steps are: poured into by aluminium lid in clean porose stainless steel framework, add in electrically heated drying cabinet, be incubated powered-down after a hour.
As mentioned above, the present invention can be realized preferably.
Claims (6)
1. the preparation technology of azlocillin sodium for injection, is characterized in that, comprises the following steps:
(1), the synthesis of azlocillin sodium: by dichloromethane and ampicillin by weight be that 1:0.064 ~ 1:0.068 mixes, regulate pH value of solution in alkalescence, obtain condensation reaction solution, under agitation put in above-mentioned condensation reaction solution by 1-Chlorocarbonyl-2-Imidazolidone, dichloromethane, the weight ratio of 1-Chlorocarbonyl-2-Imidazolidone, dichloromethane and condensation reaction solution is 1:4.5:28 ~ 1:4.8:31; PH value of solution is regulated to be alkalescence, continue to stir, obtain condensation reaction material, water is adopted to carry out successively extract and separate to above-mentioned condensation reaction material, water layer is transferred in crystallizer, with acid for adjusting pH, crystalline solid centrifugal after crystallization, crystalline solid is washed and the azlocillin of drying, azlocillin is passed under the condition of cooling medium at retort interlayer and dissolves and the water in tank, after dissolving, add sodium hydroxide solution, add sodium bicarbonate solution and regulate pH, in solution, add depigmenting agent again, after filtration, sterilizing, obtain azlocillin sodium wet product;
(2), the azlocillin sodium wet product lyophilization of synthesis is prepared into Powdered by pulverizing and sieves;
(3), the preparation technology of azlocillin sodium: first cleaning is used for the reagent bottle of splendid attire azlocillin sodium powder, then azlocillin sodium powder is quantitatively loaded the above-mentioned reagent bottle cleaned by specification and be filled with nitrogen, then pretreated plug is covered, Zha Gai process is carried out again with aluminium lid, product is sealed, interior label, packaging, lamp inspection are pasted successively to the reagent bottle after Zha Gai, then labels outer on packing box, then test, pack.
2. the preparation technology of azlocillin sodium for injection according to claim 1, is characterized in that, described dichloromethane and ampicillin are 1:0.065 by weight.
3. the preparation technology of azlocillin sodium for injection according to claim 1 and 2, is characterized in that, the weight ratio of described 1-Chlorocarbonyl-2-Imidazolidone, dichloromethane and condensation reaction solution is 1:4.6:28.5.
4. the preparation technology of azlocillin sodium for injection according to claim 1, is characterized in that, the cleaning process of described reagent bottle is followed successively by supersound washing, Shui Chong, air oven dry, oven for drying, sterilizing.
5. the preparation technology of the azlocillin sodium for injection according to claim 1 or 4, is characterized in that, the plug of described reagent bottle Zha Gai adopts rubber plug cleaning machine cleaning and sterilization treatment.
6. the preparation technology of azlocillin sodium for injection according to claim 5, it is characterized in that, described aluminium lid need pass through and process, and pretreated concrete steps are: poured into by aluminium lid in clean porose stainless steel framework, add in electrically heated drying cabinet, be incubated powered-down after a hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510200598.3A CN104771367A (en) | 2015-04-27 | 2015-04-27 | Preparation process of azlocillin sodium for injection |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510200598.3A CN104771367A (en) | 2015-04-27 | 2015-04-27 | Preparation process of azlocillin sodium for injection |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104771367A true CN104771367A (en) | 2015-07-15 |
Family
ID=53613357
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510200598.3A Pending CN104771367A (en) | 2015-04-27 | 2015-04-27 | Preparation process of azlocillin sodium for injection |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104771367A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106176215A (en) * | 2016-06-28 | 2016-12-07 | 宋占涛 | A kind of clamped bottle goods drying property and the keeping method of stability |
| CN111362969A (en) * | 2020-04-22 | 2020-07-03 | 苏州二叶制药有限公司 | Preparation process of azlocillin sodium |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102311450A (en) * | 2011-09-23 | 2012-01-11 | 江苏汉斯通药业有限公司 | Preparation method for Azlocillin sodium |
-
2015
- 2015-04-27 CN CN201510200598.3A patent/CN104771367A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102311450A (en) * | 2011-09-23 | 2012-01-11 | 江苏汉斯通药业有限公司 | Preparation method for Azlocillin sodium |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106176215A (en) * | 2016-06-28 | 2016-12-07 | 宋占涛 | A kind of clamped bottle goods drying property and the keeping method of stability |
| CN111362969A (en) * | 2020-04-22 | 2020-07-03 | 苏州二叶制药有限公司 | Preparation process of azlocillin sodium |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102670563A (en) | Preparation method of soft capsule without gelatin | |
| CN104886554A (en) | Pomander soft capsule and preparation method thereof | |
| CN104771367A (en) | Preparation process of azlocillin sodium for injection | |
| CN105079818B (en) | Florfenicol soluble powder is prepared with acetamide and cyclodextrin | |
| CN104892705A (en) | Preparation technology of tylosin tartrate for injection | |
| CN103224539A (en) | Gastrodine compound and pharmaceutical composition thereof | |
| CN104000191A (en) | A novel chelated calcium | |
| CN104771366A (en) | Preparation process of ceftriaxone sodium for injection | |
| CN102440965A (en) | Esomeprazole sodium composition used for injection and its preparation method | |
| CN103655500B (en) | A kind of VITAMIN C TABLET and preparation method thereof | |
| CN104840423A (en) | Preparation process of cefotaxime sodium for injection | |
| CN102755325B (en) | Cefoxitin sodium medicinal composition, powder injection and preparation method thereof | |
| CN100531700C (en) | Method for producing hollow capsules dissoluble in stomach by using seaweed polysaccharide as raw material | |
| CN104761569A (en) | Method for preparing azlocillin sodium for injection and facilitating rejection of non-confirming products | |
| CN104774211A (en) | Preparation technique of cefuroxime sodium for injection | |
| CN104758260A (en) | Cefoxitin sodium powder-injection for injection and preparation method of cefoxitin sodium powder-injection | |
| CN108498479A (en) | A kind of filling liquid type empty hard capsule | |
| CN105862407A (en) | Method for preparing bamboo fiber hemostatic gauze | |
| CN104784184A (en) | Preparation technology of cefotaxime sodium sulbactam sodium for injection | |
| CN108125193A (en) | A kind of preparation method of food additive citric acid iron | |
| CN1214796C (en) | Method for preparing slow release micro pill of aspirin | |
| CN104338145A (en) | Dropping pill with sodium alginate and gellan gum as capsule wall material, and its production technology | |
| CN102697753B (en) | Roxithromycin soft capsule preparation thereof | |
| CN102172352B (en) | Lipoic acid composition for injection and preparation method thereof | |
| CN102579356A (en) | Preparation method of penehyclidine hydrochloride powder injection for injecting |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150715 |