CN104840433A - Freeze drying method of omeprazole sodium for injection and omeprazole sodium for injection - Google Patents
Freeze drying method of omeprazole sodium for injection and omeprazole sodium for injection Download PDFInfo
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- CN104840433A CN104840433A CN201410817570.XA CN201410817570A CN104840433A CN 104840433 A CN104840433 A CN 104840433A CN 201410817570 A CN201410817570 A CN 201410817570A CN 104840433 A CN104840433 A CN 104840433A
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Abstract
The invention discloses a freeze drying method of omeprazole sodium for injection and omeprazole sodium for injection. A prepared omeprazole sodium liquid medicine for injection is subjected to filling and then to quick-freezing in a vacuum freezing dryer. The specific quick-freezing steps include: cooling the liquid medicine from normal temperature to -40DEG C within 1.0-1.5h and conducting heat preservation for 1.0-2.0h; at the end of quick-freezing, letting the liquid medicine enter a sublimation drying stage, raising the temperature of the product from -40DEG C to -20DEG C in 15.0-20.0 hours and conducting heat preservation for 5.0-8.0h, when the ice crystal line disappears and the sublimation drying finishes, bringing the product into a desorption drying stage, raising the temperature of the product from -20DEG C to 30DEG C in 10.0-15.0h and conducting heat preservation for 4.0-5.0h, then decreasing the temperature to normal temperature in 1.0-2.0h, and taking the product out of the box, thus finishing the freeze drying process. The omeprazole sodium for injection obtained in the invention has the advantages of qualified quality, soft appearance, no collapse or shrinkage phenomenon, good roundness, and easy solubility, and is easy to preserve.
Description
Technical field:
The present invention relates to a kind of freeze-drying method and the injection omeprazole sodium thereof of injection omeprazole sodium.
Background technology:
The method of medicine drying is more, and as microwave drying, hot-air seasoning, spraying dry and vacuum drying etc., but usual drying method all carries out usually more than 0 DEG C or at higher temperature.Generally all there is the phenomenons such as volume-diminished, quality be hardening in the product of dry gained, those volatile compositions major parts can Yin Wendu too high and lose, more have some to the material of thermal sensitivity, degeneration, inactivation, oxidation etc. can occur.Therefore, dried product, compared with before drying, character has very large difference.
Vacuum freeze-drying method then carries out substantially below 0 DEG C, carries out drying under the state namely freezed at product, only when the later stage reduces the remaining water content of product, just allows product rise to the temperature of more than 0 DEG C, but is generally no more than 30 DEG C.Under vacuum, after water vapour directly distils out, in the left skeleton when freezing of medicine, form similar Sponge Porosity porous framework, therefore its dry rear volume size is almost constant.Before reusing, as long as add water for injection, can dissolve immediately.
Injection omeprazole sodium is a kind of lyophilized formulations, has sulfinyl in the chemical constitution of Omeprazole Sodium, unstable in aqueous; therefore make freeze drying powder preparations, require to control comparatively sternly, by common production method to moisture content; cannot product quality be ensured, be unfavorable for preserving.
Summary of the invention:
One of technical problem to be solved by this invention is the freeze-drying method providing a kind of injection omeprazole sodium for the deficiency existing for the existing freeze-drying method of injection omeprazole sodium.
Two of technical problem to be solved by this invention is to provide a kind of injection omeprazole sodium.
Lyophilization principle of the present invention utilizes water to have state phase in solid-state, liquid, gaseous state three, and according to the Phase Equilibrium theory in thermodynamics, with the reduction of pressure, the freezing point change of water is little, and boiling point is more and more lower, close to freezing point.When pressure is reduced to certain vacuum, the boiling point of water and freezing point overlap, and ice just can direct boiling be gas without liquid state.Namely, under low-temp low-pressure condition, make the water sublimed freezed in medicine and slough.
The present invention contains Omeprazole Sodium less (40mg) in injection omeprazole sodium, adjuvant mannitol is mainly utilized to make skeleton, within the extremely short time, injection omeprazole sodium is frozen into solid-state, and when temperature and vacuum extremely low the solid water in injection omeprazole sodium is directly flashed to gaseous state by the form of evacuation, again the gas containing a large amount of water vapour is cooled to water to discharge, thus reaches dry object.
Technical problem to be solved by this invention can be achieved through the following technical solutions:
A kind of freeze-drying method of injection omeprazole sodium, it is frozen by entering the laggard scanning frequency of vacuum freeze drier after fill half tamponade by the injection omeprazole sodium medicinal liquid after preparation in process of production, concrete fast freezing step is: injection omeprazole sodium medicinal liquid was cooled to-40 DEG C rapidly from room temperature by medicinal liquid within 1.0 ~ 1.5 hours, and is incubated 1.0 ~ 2.0 hours at this temperature; Quick-freezing terminates directly to enter the sublimation drying stage afterwards, the described sublimation drying stage is that temperature was elevated to-20 DEG C from-40 DEG C by goods within 15.0 ~ 20.0 hours, and be incubated 5.0 ~ 8.0 hours at this temperature, until ice day heading line off sublimation drying enter the parsing-desiccation stage after terminating; The described parsing-desiccation stage is that temperature was elevated to 30 DEG C from-20 DEG C by goods within 10.0 ~ 15.0 hours, and is incubated 4.0 ~ 5.0 hours at this temperature, then within 1.0 ~ 2.0 hours, temperature is reduced to room temperature, outlet, terminates freezing dry process.
A kind of injection omeprazole sodium, is prepared from according to above-mentioned method.
Owing to have employed technical scheme as above, the injection omeprazole sodium that the present invention obtains is up-to-standard, and outward appearance is soft, steps on and atrophy phenomenon without collapsing, and roundness is better, very easily dissolves, is beneficial to preservation.
Detailed description of the invention
Concrete technical scheme and experimental procedure as follows:
1. first time test
1.1 test periods: on April 5th, 2012 was to April 7
1.2 batch numbers: 20120401
1.3 batch number titles: injection omeprazole sodium
1.4 product specifications: 40mg
1.5 test procedures:
1.5.1 configurating filtered good medicinal liquid is passed through fill half tamponade, the product 9500 bottles of half tamponade is put into freezer dryer, close freeze dryer door.
1.5.2 optimum configurations is carried out to freeze dryer:
1.5.2.1 pre-freeze optimum configurations: product cools to-40 DEG C from room temperature, required time 1.0 hours, and be incubated 1.0 hours at this temperature;
1.5.2.2 sublimation drying optimum configurations: product is warmed up to-20 DEG C from-40 DEG C, required time 10.0 hours, and be incubated 5.0 hours at this temperature;
1.5.2.3 parsing-desiccation optimum configurations: product is warmed up to 30 DEG C from-20 DEG C, required time 10.0 hours, and be incubated 4.0 hours at this temperature; Product is down to room temperature from 30 DEG C, and required time is 1.0 hours, and this temperature 1.0 hours.
1.5.3 starting device after parameter device, equipment normally runs automatically.In running, observation medicine ice crystal heading line off situation and parameters have without exception.
1.5.4 product outlet, roll and cover and carry out quality examination, quality examination situation refers to following table 1:
Table 1
2. second time test
2.1 test periods: on April 8th, 2012 was to April 10
2.2 batch number: 20120402
2.3 batch number titles: injection omeprazole sodium
2.4 product specification: 40mg
2.5 test procedures:
2.5.1 configurating filtered good medicinal liquid is passed through fill half tamponade, the product 9450 bottles of half tamponade is put into freezer dryer, close freeze dryer door.
2.5.2 carry out optimum configurations to freeze dryer:
2.5.2.1 pre-freeze optimum configurations: product cools to-42 DEG C from room temperature, required time 1.2 hours, and be incubated 1.5 hours at this temperature;
2.5.2.2 sublimation drying optimum configurations: product is warmed up to-20 DEG C from-42 DEG C, required time 12.0 hours, and be incubated 6.0 hours at this temperature;
2.5.2.3 parsing-desiccation optimum configurations: product is warmed up to 30 DEG C from-20 DEG C, required time 12.0 hours, and be incubated 4.5 hours at this temperature; Product is down to room temperature from 30 DEG C, required time 1.5 hours, and this temperature 1.0 hours.
2.5.3 starting device after parameter device, equipment normally runs automatically.In running, observation medicine ice crystal heading line off situation and parameters have without exception.
2.5.4 product outlet, roll and cover and carry out quality examination, quality examination situation refers to following table 2:
Table 2
3. third time test
3.1 test periods: on April 11st, 2012 was to April 12
3.2 batch number: 20120403
3.3 batch number titles: injection omeprazole sodium
3.4 product specification: 40mg
3.5 test procedures:
3.5.1 configurating filtered good medicinal liquid is passed through fill half tamponade, the product 9600 of half tamponade is put into freezer dryer, close freeze dryer door.
3.5.2 carry out optimum configurations to freeze dryer:
3.5.2.1 pre-freeze optimum configurations: product cools to-45 DEG C from room temperature, required time 1.5 hours, and be incubated 2.0 hours at this temperature;
3.5.2.2 sublimation drying optimum configurations: product is warmed up to-20 DEG C from-45 DEG C, required time 15.0 hours, and be incubated 8.0 hours at this temperature;
3.5.2.3 parsing-desiccation optimum configurations: product is warmed up to 30 DEG C from-20 DEG C, required time 15.0 hours, and be incubated 5.0 hours at this temperature; Product is down to room temperature from 30 DEG C, required time 2.0 hours, and this temperature 1.0 hours.
3.5.3 starting device after parameter device, equipment normally runs automatically.In running, observation medicine ice crystal heading line off situation and parameters have without exception.
3.5.4 product outlet, roll and cover and carry out quality examination, quality examination situation refers to following table 3:
Table 3
Yield contrast is in table 4
Table 4
By analyzing the test of above three batches, the conclusion injection omeprazole sodium drawn is produced under the Parameter Conditions set by test, can produce qualified product completely.
Claims (2)
1. the freeze-drying method of an injection omeprazole sodium, it is frozen by entering the laggard scanning frequency of vacuum freeze drier after fill half tamponade by the injection omeprazole sodium medicinal liquid after preparation in process of production, concrete fast freezing step is: injection omeprazole sodium medicinal liquid was cooled to-40 DEG C rapidly from room temperature by medicinal liquid within 1.0 ~ 1.5 hours, and is incubated 1.0 ~ 2.0 hours at this temperature; Quick-freezing terminates directly to enter the sublimation drying stage afterwards, the described sublimation drying stage is that temperature was elevated to-20 DEG C from-40 DEG C by goods within 15.0 ~ 20.0 hours, and be incubated 5.0 ~ 8.0 hours at this temperature, until ice day heading line off sublimation drying enter the parsing-desiccation stage after terminating; The described parsing-desiccation stage is that temperature was elevated to 30 DEG C from-20 DEG C by goods within 10.0 ~ 15.0 hours, and is incubated 4.0 ~ 5.0 hours at this temperature, then within 1.0 ~ 2.0 hours, temperature is reduced to room temperature, outlet, terminates freezing dry process.
2. an injection omeprazole sodium, is characterized in that, is prepared from according to method according to claim 1.
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| CN201410817570.XA CN104840433A (en) | 2014-12-23 | 2014-12-23 | Freeze drying method of omeprazole sodium for injection and omeprazole sodium for injection |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105919953A (en) * | 2016-06-27 | 2016-09-07 | 峨眉山通惠制药有限公司 | Omeprazole sodium composition for injection and production process of omeprazole sodium composition |
| CN107260691A (en) * | 2017-08-08 | 2017-10-20 | 湖南科伦制药有限公司 | A kind of preparation method of omeprazole freeze-dried powder injection |
| CN112807282A (en) * | 2021-01-13 | 2021-05-18 | 海南葫芦娃药业集团股份有限公司 | Omeprazole sodium freeze-dried powder injection and preparation method thereof |
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| CN101926799A (en) * | 2009-06-18 | 2010-12-29 | 刘建红 | Omeprazole sodium medicinal composition for injection and preparation method thereof |
| CN101987099A (en) * | 2009-08-07 | 2011-03-23 | 上海秀新臣邦医药科技有限公司 | Omeprazole sodium for injection and preparation method thereof |
| CN102151264A (en) * | 2011-05-10 | 2011-08-17 | 江苏奥赛康药业有限公司 | Omeprazole sodium composition for injection |
| CN103169674A (en) * | 2013-04-17 | 2013-06-26 | 成都天台山制药有限公司 | Omeprazole sodium freeze-dried powder injection for injection |
| CN103690495A (en) * | 2013-12-19 | 2014-04-02 | 贵州景峰注射剂有限公司 | Freeze drying method of naloxone hydrochloride for injection |
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2014
- 2014-12-23 CN CN201410817570.XA patent/CN104840433A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101926799A (en) * | 2009-06-18 | 2010-12-29 | 刘建红 | Omeprazole sodium medicinal composition for injection and preparation method thereof |
| CN101987099A (en) * | 2009-08-07 | 2011-03-23 | 上海秀新臣邦医药科技有限公司 | Omeprazole sodium for injection and preparation method thereof |
| CN102151264A (en) * | 2011-05-10 | 2011-08-17 | 江苏奥赛康药业有限公司 | Omeprazole sodium composition for injection |
| CN103169674A (en) * | 2013-04-17 | 2013-06-26 | 成都天台山制药有限公司 | Omeprazole sodium freeze-dried powder injection for injection |
| CN103690495A (en) * | 2013-12-19 | 2014-04-02 | 贵州景峰注射剂有限公司 | Freeze drying method of naloxone hydrochloride for injection |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105919953A (en) * | 2016-06-27 | 2016-09-07 | 峨眉山通惠制药有限公司 | Omeprazole sodium composition for injection and production process of omeprazole sodium composition |
| CN107260691A (en) * | 2017-08-08 | 2017-10-20 | 湖南科伦制药有限公司 | A kind of preparation method of omeprazole freeze-dried powder injection |
| CN112807282A (en) * | 2021-01-13 | 2021-05-18 | 海南葫芦娃药业集团股份有限公司 | Omeprazole sodium freeze-dried powder injection and preparation method thereof |
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Application publication date: 20150819 |