CN103044455B - Reworking method of cefpirome sulfate mixed powder - Google Patents
Reworking method of cefpirome sulfate mixed powder Download PDFInfo
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- CN103044455B CN103044455B CN201110313650.8A CN201110313650A CN103044455B CN 103044455 B CN103044455 B CN 103044455B CN 201110313650 A CN201110313650 A CN 201110313650A CN 103044455 B CN103044455 B CN 103044455B
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- cefpirome sulfate
- filtrate
- reworking method
- exchange resin
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Abstract
The invention discloses a reworking method of cefpirome sulfate mixed powder. The reworking method comprises the following steps of: 1) dissolving the cefpirome sulfate mixed powder to be reworked in a certain amount of water, and setting the temperature at 0 DEG C-30 DEG C; 2) enabling the solution after dissolution to pass through a column loaded with an adsorbent, and collecting filtrate; 3) adding activated carbon into the filtrate, performing decolorization reaction, and controlling the reaction time at 30min; 4) filtering and collecting the filtrate; 5) dripping a sulfuric acid solution into the filtrate, and regulating the pH value to 1.2-2.4; 6) adding a crystallizing agent into the filtrate for crystallization, controlling the crystallization temperature at 0 DEG C-30 DEG C, and stirring for 2-4h; 7) filtering to obtain a crystal after filtration, and washing with one solution or a mixed solution of acetone and alcohol; and 8) controlling the temperature at 45 DEG C-55 DEG C, and drying to obtain the cefpirome sulfate. According to the reworking method disclosed by the invention, the unqualified cefpirome sulfate can be effectively reworked and refined to produce a qualified product, and the cost can be further reduced.
Description
Technical field
The present invention relates to the reworking method that a kind of Cefpirome Sulfate mixes powder.
Background technology
Cefpirome Sulfate is forth generation broad-spectrum cephalosporin class microbiotic, there is broad-spectrum high efficacy and suppress beta-lactam enzyme viability, the clinical treatment for moderate and severe infection patient, because Cefpirome Sulfate itself is slightly soluble in water, and in acid, use after therefore and sodium carbonate general as injection use forms mixed powder clinically.Because in synthesis production, link is numerous, route is longer, expensive, occurs the color because other reasons causes in preparation process sometimes, content, impurity, aseptic, visible foreign matters etc. are defective, mix sodium carbonate and mix powder and then abandon, comparatively waste for underproof Cefpirome Sulfate.
Summary of the invention
For overcoming above-mentioned shortcoming, the object of the present invention is to provide one effectively defective Cefpirome Sulfate can be mixed powder and do over again and be refined into qualified product, and the Cefpirome Sulfate reduced costs mixing the reworking method of powder.
In order to reach above object, the technical solution used in the present invention is: a kind of Cefpirome Sulfate mixes the reworking method of powder, comprises the following steps:
1) Cefpirome Sulfate to be done over again is mixed powder and is dissolved in a certain amount of water, solvent temperature is set as 0 DEG C ~ 30 DEG C;
2), after the solution after dissolving being crossed the post that sorbent material is housed, filtrate is collected;
3) in filtrate, add gac and carry out decoloring reaction, will control in the reaction times at 30min;
4) filter, collect the filtrate after decolouring;
5) with in the filtrate after sulphuric acid soln instillation decolouring, and pH value to 1.2 ~ 2.4 are regulated;
6) in filtrate, add quantitative crystallizing agent and carry out crystallization, Tc controls at 0 DEG C ~ 30 DEG C, and stirs 2 ~ 4h;
7) filter, obtain the crystallization after filtering, and wash with the wherein a kind of solution in acetone and alcohol or mixing solutions;
8) temperature is controlled, at 45 DEG C ~ 55 DEG C, carry out drying, obtain Cefpirome Sulfate.
Preferably, described sorbent material is the one in storng-acid cation exchange resin and weakly acidic cation-exchange resin.
Preferably, described Zeo-karb is applied mechanically by hydrochloric acid soln regenerated from washing.
Preferably, described storng-acid cation exchange resin is the one in 732 type storng-acid cation exchange resins, 011 type storng-acid cation exchange resin, 001 type storng-acid cation exchange resin.
Preferably, described weakly acidic cation-exchange resin is the one in 107 type weakly acidic cation-exchange resins, 113 type weakly acidic cation-exchange resins.
Preferably, the quality of described crystallizing agent is 10 ~ 35 times that Cefpirome Sulfate to be done over again mixes the quality of powder.
Owing to have employed technique scheme, defective Cefpirome Sulfate can be mixed powder and do over again and be refined into qualified product by the present invention effectively, and the Cefpirome Sulfate reduced costs mixes the reworking method of powder.
Embodiment
Below preferred embodiment of the present invention is described in detail, can be easier to make advantages and features of the invention be readily appreciated by one skilled in the art, thus more explicit defining is made to protection scope of the present invention.
The invention provides the reworking method that a kind of Cefpirome Sulfate mixes powder, it is characterized in that, comprise the following steps:
1) Cefpirome Sulfate to be done over again is mixed powder and is dissolved in a certain amount of water, solvent temperature is set as 0 DEG C ~ 30 DEG C;
2), after the solution after dissolving being crossed the post that sorbent material is housed, filtrate is collected;
3) in filtrate, add gac and carry out decoloring reaction, will control in the reaction times at 30min;
4) filter, collect the filtrate after decolouring;
5) with in the filtrate after sulphuric acid soln instillation decolouring, and pH value to 1.2 ~ 2.4 are regulated;
6) in filtrate, add quantitative crystallizing agent and carry out crystallization, and stir 2 ~ 4h;
7) filter, obtain the crystallization after filtering, and wash with the wherein a kind of solution in acetone and alcohol or mixing solutions;
8) temperature is controlled, at 45 DEG C ~ 55 DEG C, carry out drying, obtain Cefpirome Sulfate.
Wherein, sorbent material is the one in storng-acid cation exchange resin and weakly acidic cation-exchange resin, Zeo-karb is applied mechanically by hydrochloric acid soln regenerated from washing, storng-acid cation exchange resin is 732 type storng-acid cation exchange resins, 011 type storng-acid cation exchange resin, one in 001 type storng-acid cation exchange resin, weakly acidic cation-exchange resin is 107 type weakly acidic cation-exchange resins, one in 113 type weakly acidic cation-exchange resins, the quality of crystallizing agent is 10 ~ 35 times that Cefpirome Sulfate to be done over again mixes the quality of powder.
Embodiment 1
The Cefpirome Sulfate to be done over again of 20g is mixed powder to be dissolved in 120ml water, solution after dissolving is crossed 732 type Zeo-karbs, collect 160ml filtrate, in filtrate, add 1g gac carry out decoloring reaction, to control in the reaction times at 30min, filter, filtrate sulphuric acid soln regulates PH to optimal values PH to be 1.6 ~ 2.0, add acetone and carry out crystallization, temperature of reaction during crystallization control is at 18 DEG C ~ 22 DEG C, and stir 2 ~ 4h, terminate reaction, filter, obtain the crystallization after filtering, with the crystallization after acetone mixture washing and filtering, qualified to moisture 45 ~ 55 DEG C of vacuum-dryings, obtain Cefpirome Sulfate 15.6g, the rate of recovery that Cefpirome Sulfate to be done over again mixes powder can reach 78.0%.
Embodiment 2
The Cefpirome Sulfate to be done over again of 20g is mixed powder to be dissolved in 120ml water, solution after dissolving is crossed 107 type Zeo-karbs, collect 160ml filtrate, in filtrate, add 1g gac carry out decoloring reaction, to control in the reaction times at 30min, filtrate sulphuric acid soln regulates PH to optimal values PH to be 1.6 ~ 2.0, add alcohol and carry out crystallization, temperature of reaction during crystallization control is at 18 DEG C ~ 22 DEG C, and stir 2 ~ 4h, terminate reaction, filter, obtain the crystallization after filtering, with the crystallization after acetone mixture washing and filtering, qualified to moisture 45 ~ 55 DEG C of vacuum-dryings, obtain Cefpirome Sulfate 16.0g, the rate of recovery that Cefpirome Sulfate to be done over again mixes powder can reach 80.0%.
Above embodiment is only for illustrating technical conceive of the present invention and feature; its object is to allow person skilled in the art understand content of the present invention and to be implemented; can not limit the scope of the invention with this; all equivalences done according to spirit of the present invention change or modify, and all should be encompassed in protection scope of the present invention.
Claims (5)
1. Cefpirome Sulfate mixes a reworking method for powder, it is characterized in that, comprises the following steps:
1) Cefpirome Sulfate to be done over again is mixed powder and is dissolved in a certain amount of water, solvent temperature is set as 0 DEG C ~ 30 DEG C;
2), after the solution after dissolving being crossed the post that sorbent material is housed, collect filtrate, described sorbent material is the one in storng-acid cation exchange resin and weakly acidic cation-exchange resin;
3) in filtrate, add gac and carry out decoloring reaction, will control in the reaction times at 30min;
4) filter, collect the filtrate after decolouring;
5) with in the filtrate after sulphuric acid soln instillation decolouring, and PH value to 1.2 ~ 2.4 are regulated;
6) in filtrate, add quantitative crystallizing agent and carry out crystallization, Tc controls at 0 DEG C ~ 30 DEG C, and stirs 2 ~ 4h;
7) filter, obtain the crystallization after filtering, and wash with the wherein a kind of solution in acetone and alcohol or mixing solutions;
8) temperature is controlled, at 45 DEG C ~ 55 DEG C, carry out drying, obtain Cefpirome Sulfate.
2. mix the reworking method of powder according to the Cefpirome Sulfate described in claim 1, it is characterized in that: described Zeo-karb is applied mechanically by hydrochloric acid soln regenerated from washing.
3. mix the reworking method of powder according to the Cefpirome Sulfate described in claim 1, it is characterized in that: described storng-acid cation exchange resin is the one in 732 type storng-acid cation exchange resins, 011 type storng-acid cation exchange resin, 001 type storng-acid cation exchange resin.
4. mix the reworking method of powder according to the Cefpirome Sulfate described in claim 1, it is characterized in that: described weakly acidic cation-exchange resin is the one in 107 type weakly acidic cation-exchange resins, 113 type weakly acidic cation-exchange resins.
5. mix the reworking method of powder according to the Cefpirome Sulfate described in claim 1, it is characterized in that: the quality of described crystallizing agent is 10 ~ 35 times that Cefpirome Sulfate to be done over again mixes the quality of powder.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110313650.8A CN103044455B (en) | 2011-10-17 | 2011-10-17 | Reworking method of cefpirome sulfate mixed powder |
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| CN201110313650.8A CN103044455B (en) | 2011-10-17 | 2011-10-17 | Reworking method of cefpirome sulfate mixed powder |
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| CN103044455A CN103044455A (en) | 2013-04-17 |
| CN103044455B true CN103044455B (en) | 2015-04-01 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103360412B (en) * | 2013-06-08 | 2015-08-19 | 苏州中联化学制药有限公司 | A kind of synthetic method of S 578 |
| CN108707158B (en) * | 2018-06-14 | 2020-01-21 | 华北制药河北华民药业有限责任公司 | Method for purifying cefpirome sulfate |
Citations (5)
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|---|---|---|---|---|
| US4609653A (en) * | 1982-12-28 | 1986-09-02 | Hoechst Aktiengesellschaft | Crystalline cephem-acid addition salts and processes for their preparation |
| CN1587267A (en) * | 2004-06-29 | 2005-03-02 | 魏雪纹 | Process for synthesizing cefpirome sulfate |
| CN101066974A (en) * | 2007-04-20 | 2007-11-07 | 苏州中联化学制药有限公司 | Synthesis process of cefpirome sulfate as antibiotic |
| CN101172982A (en) * | 2006-11-03 | 2008-05-07 | 河北凯盛医药科技有限公司 | Method of preparing cefpirome sulfate |
| CN101362770A (en) * | 2007-08-10 | 2009-02-11 | 上海新先锋药业有限公司 | Cefpirome sulfate preparation technology |
-
2011
- 2011-10-17 CN CN201110313650.8A patent/CN103044455B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4609653A (en) * | 1982-12-28 | 1986-09-02 | Hoechst Aktiengesellschaft | Crystalline cephem-acid addition salts and processes for their preparation |
| CN1587267A (en) * | 2004-06-29 | 2005-03-02 | 魏雪纹 | Process for synthesizing cefpirome sulfate |
| CN101172982A (en) * | 2006-11-03 | 2008-05-07 | 河北凯盛医药科技有限公司 | Method of preparing cefpirome sulfate |
| CN101066974A (en) * | 2007-04-20 | 2007-11-07 | 苏州中联化学制药有限公司 | Synthesis process of cefpirome sulfate as antibiotic |
| CN101362770A (en) * | 2007-08-10 | 2009-02-11 | 上海新先锋药业有限公司 | Cefpirome sulfate preparation technology |
Non-Patent Citations (2)
| Title |
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| 硫酸头孢匹罗的合成;宋艳玲等;《沈阳化工大学学报》;20110930;第25卷(第3期);225-228 * |
| 硫酸头孢匹罗的合成工艺改进;刘洪雨等;《中国抗生素杂志》;20090228;第32卷(第2期);87-89 * |
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Address after: 215212 No. 6 Jinzi Road, Lili Town, Wujiang District, Suzhou City, Jiangsu Province Patentee after: Suzhou Shengda Pharmaceutical Co., Ltd. Address before: 215212 No. 9 Jiaotong East Road, Lili Town, Wujiang City, Jiangsu Province Patentee before: China Union Chempharma (Suzhou) Co., Ltd. |
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