CN103044455A - Reworking method of cefpirome sulfate mixed powder - Google Patents
Reworking method of cefpirome sulfate mixed powder Download PDFInfo
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- CN103044455A CN103044455A CN2011103136508A CN201110313650A CN103044455A CN 103044455 A CN103044455 A CN 103044455A CN 2011103136508 A CN2011103136508 A CN 2011103136508A CN 201110313650 A CN201110313650 A CN 201110313650A CN 103044455 A CN103044455 A CN 103044455A
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- cefpirome sulfate
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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 of the mixed powder of a kind of Cefpirome Sulfate.
Background technology
Cefpirome Sulfate be the 4th generation broad-spectrum cephalosporin class microbiotic, has the characteristic that broad-spectrum high efficacy suppresses β-lactamase, clinical treatment for moderate and severe infection patient, because Cefpirome Sulfate itself is slightly soluble in water, and be acid, use after therefore and yellow soda ash general as the injection use forms mixed powder clinically.Because link is numerous in synthetic production, route is longer, and is expensive, occurs sometimes the color that causes because of other reasons in the preparation process, content, impurity, aseptic, visible foreign matters etc. are defective, then abandon comparatively waste for the mixed powder of the mixed yellow soda ash of underproof Cefpirome Sulfate.
Summary of the invention
For overcoming above-mentioned shortcoming, the object of the present invention is to provide a kind of can effectively the mixed powder of defective Cefpirome Sulfate being done over again to be refined into qualified product, and reduce the reworking method of the mixed powder of Cefpirome Sulfate of cost.
In order to reach above purpose, the technical solution used in the present invention is: the reworking method of the mixed powder of a kind of Cefpirome Sulfate may further comprise the steps:
1) the mixed powder of Cefpirome Sulfate to be done over again is dissolved in a certain amount of water, solvent temperature is set as 0 ℃～30 ℃;
2) after the solution after will dissolving is crossed the post that sorbent material is housed, collect filtrate;
3) in filtrate, add gac and carry out decoloring reaction, will the reaction times be controlled at 30min;
4) filter, collect the filtrate after decolouring;
5) splash in the filtrate after the decolouring with sulphuric acid soln, and regulate pH value to 1.2～2.4;
6) add quantitative crystallizing agent in filtrate and carry out crystallization, Tc is controlled at 0 ℃～30 ℃, and stirs 2～4h;
7) filter, the crystallization after obtaining filtering, and wash with the wherein a kind of solution in acetone and the alcohol or mixing solutions;
8) temperature is controlled at 45 ℃～55 ℃, carries out drying, obtain Cefpirome Sulfate.
Preferably, described sorbent material is a kind of in storng-acid cation exchange resin and the weakly acidic cation-exchange resin.
Preferably, described Zeo-karb is applied mechanically by the hydrochloric acid soln regenerated from washing.
Preferably, described storng-acid cation exchange resin is a kind of in 732 type storng-acid cation exchange resins, 011 type storng-acid cation exchange resin, the 001 type storng-acid cation exchange resin.
Preferably, described weakly acidic cation-exchange resin is a kind of in 107 type weakly acidic cation-exchange resins, the 113 type weakly acidic cation-exchange resins.
Preferably, the quality of described crystallizing agent is 10～35 times of quality of the mixed powder of Cefpirome Sulfate to be done over again.
Owing to having adopted technique scheme, the present invention can effectively do over again the mixed powder of defective Cefpirome Sulfate and be refined into qualified product, and reduces the reworking method of the mixed powder of Cefpirome Sulfate of cost.
Embodiment
The below is described in detail preferred embodiment of the present invention, thereby so that advantages and features of the invention can be easier to be it will be appreciated by those skilled in the art that protection scope of the present invention is made more explicit defining.
The invention provides the reworking method of the mixed powder of a kind of Cefpirome Sulfate, it is characterized in that, may further comprise the steps:
1) the mixed powder of Cefpirome Sulfate to be done over again is dissolved in a certain amount of water, solvent temperature is set as 0 ℃～30 ℃;
2) after the solution after will dissolving is crossed the post that sorbent material is housed, collect filtrate;
3) in filtrate, add gac and carry out decoloring reaction, will the reaction times be controlled at 30min;
4) filter, collect the filtrate after decolouring;
5) splash in the filtrate after the decolouring with sulphuric acid soln, and regulate pH value to 1.2～2.4;
6) in filtrate, add quantitative crystallizing agent and carry out crystallization, and stir 2～4h;
7) filter, the crystallization after obtaining filtering, and wash with the wherein a kind of solution in acetone and the alcohol or mixing solutions;
8) temperature is controlled at 45 ℃～55 ℃, carries out drying, obtain Cefpirome Sulfate.
Wherein, sorbent material is a kind of in storng-acid cation exchange resin and the weakly acidic cation-exchange resin, Zeo-karb is applied mechanically by the 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, a kind of in the 001 type storng-acid cation exchange resin, weakly acidic cation-exchange resin is 107 type weakly acidic cation-exchange resins, a kind of in the 113 type weakly acidic cation-exchange resins, the quality of crystallizing agent is 10～35 times of quality of the mixed powder of Cefpirome Sulfate to be done over again.
Embodiment 1
The mixed powder of the Cefpirome Sulfate to be done over again of 20g is dissolved in the 120ml water, solution after the dissolving is crossed 732 type Zeo-karbs, collect 160ml filtrate, in filtrate, add the 1g gac and carry out decoloring reaction, to the reaction times be controlled at 30min, filter, filtrate with sulphuric acid soln regulate PH to optimal values PH be 1.6～2.0, add acetone and carry out crystallization, temperature of reaction during crystallization control is at 18 ℃～22 ℃, and stirs 2～4h, finishes reaction, filter, crystallization after obtaining filtering, with the crystallization behind the acetone mixed solution washing and filtering, qualified to moisture 45～55 ℃ of vacuum-dryings, get Cefpirome Sulfate 15.6g, the rate of recovery of the mixed powder of Cefpirome Sulfate to be done over again can reach 78.0%.
Embodiment 2
The mixed powder of the Cefpirome Sulfate to be done over again of 20g is dissolved in the 120ml water, solution after the dissolving is crossed 107 type Zeo-karbs, collect 160ml filtrate, in filtrate, add the 1g gac and carry out decoloring reaction, to the reaction times be controlled at 30min, filtrate with sulphuric acid soln regulate PH to optimal values PH be 1.6～2.0, add alcohol and carry out crystallization, temperature of reaction during crystallization control is at 18 ℃～22 ℃, and stir 2～4h, finish reaction, filter the crystallization after obtaining filtering, with the crystallization behind the acetone mixed solution washing and filtering, qualified to moisture 45～55 ℃ of vacuum-dryings, get Cefpirome Sulfate 16.0g, the rate of recovery of the mixed powder of Cefpirome Sulfate to be done over again can reach 80.0%.
Above embodiment only is explanation technical conceive of the present invention and characteristics; its purpose is to allow the people that is familiar with technique understand content of the present invention and is implemented; can not limit protection scope of the present invention with this; all equivalences that spirit is done according to the present invention change or modify, and all should be encompassed in protection scope of the present invention.
Claims (6)
1. the reworking method of the mixed powder of Cefpirome Sulfate is characterized in that, may further comprise the steps:
1) the mixed powder of Cefpirome Sulfate to be done over again is dissolved in a certain amount of water, solvent temperature is set as 0 ℃～30 ℃;
2) after the solution after will dissolving is crossed the post that sorbent material is housed, collect filtrate;
3) in filtrate, add gac and carry out decoloring reaction, will the reaction times be controlled at 30min;
4) filter, collect the filtrate after decolouring;
5) splash in the filtrate after the decolouring with sulphuric acid soln, and regulate pH value to 1.2～2.4;
6) add quantitative crystallizing agent in filtrate and carry out crystallization, Tc is controlled at 0 ℃～30 ℃, and stirs 2～4h;
7) filter, the crystallization after obtaining filtering, and wash with the wherein a kind of solution in acetone and the alcohol or mixing solutions;
8) temperature is controlled at 45 ℃～55 ℃, carries out drying, obtain Cefpirome Sulfate.
2. the reworking method of the mixed powder of Cefpirome Sulfate according to claim 1 is characterized in that: described sorbent material is a kind of in storng-acid cation exchange resin and the weakly acidic cation-exchange resin.
3. Cefpirome Sulfate according to claim 2 mixes the reworking method of powder, and it is characterized in that: described Zeo-karb is applied mechanically by the hydrochloric acid soln regenerated from washing.
4. the reworking method of the mixed powder of Cefpirome Sulfate according to claim 2 is characterized in that: described storng-acid cation exchange resin is a kind of in 732 type storng-acid cation exchange resins, 011 type storng-acid cation exchange resin, the 001 type storng-acid cation exchange resin.
5. the reworking method of the mixed powder of Cefpirome Sulfate according to claim 2 is characterized in that: described weakly acidic cation-exchange resin is a kind of in 107 type weakly acidic cation-exchange resins, the 113 type weakly acidic cation-exchange resins.
6. the reworking method of the mixed powder of Cefpirome Sulfate according to claim 1 is characterized in that: the quality of described crystallizing agent is 10～35 times of quality of the mixed powder of Cefpirome Sulfate to be done over again.
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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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| CN103044455B CN103044455B (en) | 2015-04-01 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103360412A (en) * | 2013-06-08 | 2013-10-23 | 苏州中联化学制药有限公司 | A kind of synthetic method of S 578 |
| CN108707158A (en) * | 2018-06-14 | 2018-10-26 | 华北制药河北华民药业有限责任公司 | A kind of purification process of Cefpirome Sulfate |
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| 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 |
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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 |
| 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 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103360412A (en) * | 2013-06-08 | 2013-10-23 | 苏州中联化学制药有限公司 | A kind of synthetic method of S 578 |
| 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 |
| CN108707158A (en) * | 2018-06-14 | 2018-10-26 | 华北制药河北华民药业有限责任公司 | A kind of purification process of Cefpirome Sulfate |
| 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 |
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| CN103044455B (en) | 2015-04-01 |
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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. |