CN104337768A - Preparation method of cefotiam hydrochloride for injection - Google Patents
Preparation method of cefotiam hydrochloride for injection Download PDFInfo
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- CN104337768A CN104337768A CN201410434457.3A CN201410434457A CN104337768A CN 104337768 A CN104337768 A CN 104337768A CN 201410434457 A CN201410434457 A CN 201410434457A CN 104337768 A CN104337768 A CN 104337768A
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- cefotiam
- cefotiam hydrochloride
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Abstract
The invention discloses a preparation method of cefotiam hydrochloride for injection. A recrystallization method is adopted, an appropriate reagent is selected for carrying out soaking treatment, and high-purity cefotiam hydrochloride can be prepared. The preparation method of cefotiam hydrochloride for injection has the advantages that technology is simple and technological conditions are strictly controlled, so that a pharmaceutical preparation with high stability and good quality can be obtained.
Description
Technical field
The present invention relates to field of medicaments, particularly, relate to the preparation method of cefotiam hydrochloridefor inj.
Background technology
Cefotiam hydrochloridefor inj, indication is be mainly used in the staphylococcus to this product sensitivity, Streptococcus (except enterococcus), streptococcus pneumoniae, hemophilus influenza, escherichia coli, Kleb, intestinal Pseudomonas, citrobacter belongs to, proteus mirabilis, proteus vulgaris, Proteus rettgeri, the caused following infection such as Morganella: septicemia, postoperative infection, burn infection, subcutaneous abscess, swelling, furuncle, furuncle and phyma, osteomyelitis, suppurative arthritis, tonsillitis (peritonsillitis, peritonsillar abscess), bronchitis, concurrent infection of bronchiectasis, pneumonia, pulmonary suppuration disease, empyema, cholangitis, cholecystitis, peritonitis, pyelonephritis, cystitis, urethritis, prostatitis, meningitis, endometritis, pelvic inflammatory disease, parametritis, adnexitis, bartholinitis, otitis media, nasal sinusitis.
The stable not in blood and phenomenon also having acetone to exceed standard of existing cefotiam hydrochloridefor inj occurs, has badly influenced its effect clinically, also can damage human body to while human tolerance's deficiency.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of cefotiam hydrochloridefor inj, this preparation method adopts the method for recrystallization and selects suitable reagent to carry out immersion treatment, the cefotiam hydrochloride that purity is high can be obtained, and cefotiam hydrochloride regulating the spleen and stomach acetone also can not exceed standard, and ensure that the problem of human administration's stability and safety.
The present invention's adopted technical scheme that solves the problem is:
The preparation method of cefotiam hydrochloridefor inj, comprises the following steps:
(1) after cefotiam hydrochloride crude product is added in sterilized water carrying out dissolving completely, add active carbon again to decolour, vacuum filtration is carried out after decolouring, with filter paper elimination active carbon, again with the impurity on membrane filtration removing cefotiam hydrochloride crude product, carry out washing to obtain cefotiam hydrochloride filtrate with ethanol water during filtration;
(2) the cefotiam hydrochloride filtrate after filtration is dripped appropriate acetone dissolved agent while stirring, control temperature is at 18-25 DEG C, mixing speed, at 210-215r/min, during a small amount of crystal to appear, leaves standstill 30-60min, continue again to stir, mixing speed, at 202-208r/min, when a large amount of crystal occurs, adds after butanols or propanol soak completely, solution is carried out vacuum filtration, obtains the cefotiam hydrochloride refined;
(3) be that after the natrium carbonicum calcinatum of 1:2 and anhydrous sodium bicarbonate and cefotiam hydrochloride carry out mixed powder process, subpackage obtains cefotiam hydrochloridefor inj by mol ratio.
By weight, described cefotiam hydrochloride is 500 parts, and natrium carbonicum calcinatum is 121 parts.
The butanols added or the volume of propanol are 20-60 times of cefotiam hydrochloride filtrate volume.
The butanols added or the volume of propanol are 40-50 times of cefotiam hydrochloride filtrate volume.
To sum up, the invention has the beneficial effects as follows:
1, the present invention adopts the mode of recrystallization, and the process conditions of strict crystallization control obtain the cefotiam hydrochloride that stability is high;
2, the present invention adopts suitable solvent to soak cefotiam hydrochloride, the amount of acetone can be controlled within safety range 0.5%.
Detailed description of the invention
Below in conjunction with embodiment, to the detailed description further of the present invention's do, but embodiments of the present invention are not limited thereto.
Embodiment 1
The preparation method of cefotiam hydrochloridefor inj, comprises the following steps:
(1) after cefotiam hydrochloride crude product is added in sterilized water carrying out dissolving completely, add active carbon again to decolour, vacuum filtration is carried out after decolouring, with filter paper elimination active carbon, again with the impurity on membrane filtration removing cefotiam hydrochloride crude product, carry out washing to obtain cefotiam hydrochloride filtrate with ethanol water during filtration;
(2) the cefotiam hydrochloride filtrate after filtration is dripped appropriate acetone dissolved agent while stirring, control temperature is at 18-25 DEG C, mixing speed, at 210-215r/min, during a small amount of crystal to appear, leaves standstill 30-60min, continue again to stir, mixing speed, at 202-208r/min, when a large amount of crystal occurs, adds after butanols or propanol soak completely, solution is carried out vacuum filtration, obtains the cefotiam hydrochloride refined;
(3) be that after the natrium carbonicum calcinatum of 1:2 and anhydrous sodium bicarbonate and cefotiam hydrochloride carry out mixed powder process, subpackage obtains cefotiam hydrochloridefor inj by mol ratio.
By weight, described cefotiam hydrochloride is 500 parts, and natrium carbonicum calcinatum is 121 parts.
The butanols added or the volume of propanol are 20 times of cefotiam hydrochloride filtrate volume.Cefotiam hydrochloride purity is 88.0%, and amounts of acetone is 0.50%.
Embodiment 2
Similar with embodiment 1, difference is:
The butanols added or the volume of propanol are 45 times of cefotiam hydrochloride filtrate volume.Cefotiam hydrochloride purity is 88.0%, and amounts of acetone is 0.45%.
Embodiment 3
Similar with embodiment 1, difference is:
The butanols added or the volume of propanol are 60 times of cefotiam hydrochloride filtrate volume.Cefotiam hydrochloride purity is 88.0%, and amounts of acetone is 0.50%.
Embodiment 4
Similar with embodiment 1, difference is:
The butanols added or the volume of propanol are 40 times of cefotiam hydrochloride filtrate volume.Cefotiam hydrochloride purity is 88.0%, and amounts of acetone is 0.48%.
Embodiment 5
Similar with embodiment 1, difference is:
The butanols added or the volume of propanol are 50 times of cefotiam hydrochloride filtrate volume.Cefotiam hydrochloride purity is 88.0%, and amounts of acetone is 0.49%.
As mentioned above, the present invention can be realized preferably.
Claims (4)
1. the preparation method of cefotiam hydrochloridefor inj, is characterized in that, comprises the following steps
Cefotiam hydrochloride crude product is added in sterilized water after carrying out dissolving completely, add active carbon again to decolour, vacuum filtration is carried out after decolouring, with filter paper elimination active carbon, again with the impurity on membrane filtration removing cefotiam hydrochloride crude product, carry out washing to obtain cefotiam hydrochloride filtrate with ethanol water during filtration;
Cefotiam hydrochloride filtrate after filtering is dripped appropriate acetone dissolved agent while stirring, control temperature is at 18-25 DEG C, mixing speed is at 210-215r/min, when a large amount of crystal occurs, add after butanols or propanol soak completely, solution is carried out vacuum filtration, obtains the cefotiam hydrochloride refined;
Be that after the natrium carbonicum calcinatum of 1:2 and anhydrous sodium bicarbonate and cefotiam hydrochloride carry out mixed powder process, subpackage obtains cefotiam hydrochloridefor inj by mol ratio.
2. the preparation method of cefotiam hydrochloridefor inj according to claim 1, is characterized in that, by weight, described cefotiam hydrochloride is 500 parts, and natrium carbonicum calcinatum is 121 parts.
3. the preparation method of cefotiam hydrochloridefor inj according to claim 1, is characterized in that, the butanols added or the volume of propanol are 20-60 times of cefotiam hydrochloride filtrate volume.
4. the preparation method of cefotiam hydrochloridefor inj according to claim 3, is characterized in that, the butanols added or the volume of propanol are 40-50 times of cefotiam hydrochloride filtrate volume.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410434457.3A CN104337768B (en) | 2014-08-29 | 2014-08-29 | The preparation method of cefotiam hydrochloridefor injection |
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| CN201410434457.3A CN104337768B (en) | 2014-08-29 | 2014-08-29 | The preparation method of cefotiam hydrochloridefor injection |
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| CN104337768A true CN104337768A (en) | 2015-02-11 |
| CN104337768B CN104337768B (en) | 2016-08-24 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104926835A (en) * | 2015-06-24 | 2015-09-23 | 山东罗欣药业集团股份有限公司 | Cefotiam hydrochloride compound, method for preparing same and pharmaceutical composition with cefotiam hydrochloride compound |
| CN109336906A (en) * | 2018-11-21 | 2019-02-15 | 山东罗欣药业集团股份有限公司 | A kind of cefotiam chloride drying process |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746324A (en) * | 2012-07-26 | 2012-10-24 | 刘全胜 | Purification method of cefotiam hydrochloride and aseptic powder injection of cefotiam hydrochloride |
| CN102190667B (en) * | 2011-03-24 | 2013-05-29 | 海南灵康制药有限公司 | New method for purifying cefotiam hydrochloride |
| CN103288853A (en) * | 2012-02-22 | 2013-09-11 | 北京博时安泰科技发展有限公司 | Novel preparation technology of cefotiam hexetil hydrochloride |
| CN103446047A (en) * | 2013-09-11 | 2013-12-18 | 杭州通盛医药科技有限公司 | Cefotiam hydrochloride pharmaceutical composition for injection and preparation method thereof |
-
2014
- 2014-08-29 CN CN201410434457.3A patent/CN104337768B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102190667B (en) * | 2011-03-24 | 2013-05-29 | 海南灵康制药有限公司 | New method for purifying cefotiam hydrochloride |
| CN103288853A (en) * | 2012-02-22 | 2013-09-11 | 北京博时安泰科技发展有限公司 | Novel preparation technology of cefotiam hexetil hydrochloride |
| CN102746324A (en) * | 2012-07-26 | 2012-10-24 | 刘全胜 | Purification method of cefotiam hydrochloride and aseptic powder injection of cefotiam hydrochloride |
| CN103446047A (en) * | 2013-09-11 | 2013-12-18 | 杭州通盛医药科技有限公司 | Cefotiam hydrochloride pharmaceutical composition for injection and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104926835A (en) * | 2015-06-24 | 2015-09-23 | 山东罗欣药业集团股份有限公司 | Cefotiam hydrochloride compound, method for preparing same and pharmaceutical composition with cefotiam hydrochloride compound |
| CN109336906A (en) * | 2018-11-21 | 2019-02-15 | 山东罗欣药业集团股份有限公司 | A kind of cefotiam chloride drying process |
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| CN104337768B (en) | 2016-08-24 |
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