Cefazolin sodium compound prepared according to novel intelligent crystallization technology and preparation of cefazolin sodium compound

A technology of cefazolin sodium and its compounds, which is applied in the field of cefazolin sodium compounds and its preparations, can solve the problems of dark color and cefazolin sodium with many impurities, and achieve high separation efficiency, short crystallization time and high crystallization efficiency Effect

Inactive Publication Date: 2017-02-22
陕西顿斯制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The first purpose of the present invention is to solve the problems of existing cefazolin sodium with many impurities and dark color, aiming at simplifying the process and improving efficiency, and providing a cefazolin sodium compound pr

Method used

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  • Cefazolin sodium compound prepared according to novel intelligent crystallization technology and preparation of cefazolin sodium compound
  • Cefazolin sodium compound prepared according to novel intelligent crystallization technology and preparation of cefazolin sodium compound
  • Cefazolin sodium compound prepared according to novel intelligent crystallization technology and preparation of cefazolin sodium compound

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Experimental program
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Effect test

Embodiment 1

[0047] The preparation of embodiment 1 cefazolin sodium compound

[0048] use attached figure 1 The equipment prepares cefazolin sodium compound.

[0049] (1) Take by weighing 5.06 kg of cefazolin sodium crude product with a purity of 87.6% and place it in the extraction tank, add 50 kg of mixed solvent of 40% ethanol water, control the temperature at 45° C., and stir to dissolve it;

[0050] (2) Pump in CO with a high-pressure liquid pump 2 Fluid to 10Mpa, stir, and maintain the pressure and temperature for 10 minutes, turn off the high pressure pump;

[0051] (3) Place crystal seeds in the crystallization pool, raise the height of the extraction pool to 30cm, open the quick interface of the two pools, let the liquid in the extraction pool enter the crystallization pool, and close the quick interface;

[0052] (4) Adjust the pressure in the crystallization tank to 0.5Mpa, the temperature is 10°C, and keep the temperature and pressure for 30 minutes;

[0053] (5) After the...

Embodiment 2

[0055] The preparation of embodiment 2 cefazolin sodium compound

[0056] use attached figure 1 The equipment prepares cefazolin sodium compound.

[0057] (1) Take by weighing 6.22 kg of cefazolin sodium crude product with a purity of 87.6% and place it in the extraction tank, add 60 kg of mixed solvent of 70% ethanol water, control the temperature at 55° C., and stir to dissolve it;

[0058] (2) Pump in CO with a high-pressure liquid pump 2 Fluid to 30Mpa, stir, and maintain the pressure and temperature for 20 minutes, turn off the high pressure pump;

[0059] (3) Place crystal seeds in the crystallization pool, raise the height of the extraction pool to 30cm, open the quick interface of the two pools, let the liquid in the extraction pool enter the crystallization pool, and close the quick interface;

[0060] (4) Regulate the pressure in the crystallization tank to be 0.5Mpa, the temperature is 20°C, and keep the temperature and pressure for 60 minutes;

[0061] (5) Afte...

Embodiment 3

[0063] The preparation of embodiment 3 cefazolin sodium compounds

[0064] use attached figure 1 The equipment prepares cefazolin sodium compound.

[0065] (1) Take by weighing 6.09 kg of cefazolin sodium crude product with a purity of 87.6% and place it in the extraction tank, add 70 kg of mixed solvent of 60% ethanol water, control the temperature at 50° C., and stir to dissolve it;

[0066] (2) Pump in CO with a high-pressure liquid pump 2 Fluid to 20Mpa, stir, and maintain the pressure and temperature for 15 minutes, turn off the high pressure pump;

[0067] (3) Place crystal seeds in the crystallization pool, raise the height of the extraction pool to 30cm, open the quick interface of the two pools, let the liquid in the extraction pool enter the crystallization pool, and close the quick interface;

[0068] (4) Adjust the pressure in the crystallization tank to be 6Mpa, the temperature is 15°C, and keep this temperature and pressure for 40 minutes;

[0069] (5) After ...

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Abstract

The invention discloses a cefazolin sodium compound prepared according to a novel intelligent crystallization technology and a preparation of the cefazolin sodium compound. 'Research, development and industrialization projects of high-end medical product refined crystallization technologies' won second prize of 2015th National Science and Technology Progress Award, and the novel intelligent crystallization technology is among the high-end medical product refined crystallization technologies. The cefazolin sodium compound is determined through X-ray powder diffraction, and main characteristic peaks represented by diffraction angles 2theta in an atlas are 12.24+-0.2 degrees, 16.23+-0.2 degrees, 18.94+-0.2 degrees, 19.26+-0.2 degrees, 19.80+-0.2 degrees, 20.61+-0.2 degrees, 21.05+-0.2 degrees and 23.57+-0.2degrees. Cefazolin sodium is recrystallized by combining a supercritical fluid extraction technology with a traditional crystallization technology. In a whole crystallization system, the process including extraction, adsorption, crystallization and drying is completed to recrystallize the cefazolin sodium at a specific temperature and at specific pressure under the joint action of supercritical fluid, a solvent, an extraction pond and a crystallizing pond. The preparation technology is high in separation efficiency with few impurities, so that preparation product quality is greatly improved.

Description

technical field [0001] The invention relates to a cefazolin sodium compound prepared by a novel intelligent crystallization technology and a preparation thereof, belonging to the technical field of medicine. Background technique [0002] The R&D and industrialization project of refined crystallization technology for high-end pharmaceutical products of one of the inventors, Tianjin University and Xi'an Lijun Pharmaceutical Co., Ltd., won the second prize of the 2015 National Science and Technology Progress Award. [0003] The new intelligent crystallization technology belongs to one of the refined crystallization technologies for high-end pharmaceutical products. It aims to break through the blockade of related pharmaceutical product crystal forms and crystallization technology patents at home and abroad, and realize a leap in the level of high-end pharmaceutical product research and development and crystallization technology. The international leading level has promoted the s...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/12A61K31/546A61P31/04A61K9/14
CPCA61K9/0019A61K9/14C07B2200/13C07D501/12C07D501/36Y02P20/54
Inventor 王坤
Owner 陕西顿斯制药有限公司
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