Cefoperazone sodium compound prepared by using fluid mechanics principle and preparation comprising cefoperazone sodium compound

A kind of technology of cefoperazone sodium and compound, which is applied in the field of cefoperazone sodium compound and its preparation, and can solve problems such as potential safety hazard

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

At present, the above-mentioned problems are still common in domestic marketed products, which make patients have certain safety hazards when taking medication.

Method used

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  • Cefoperazone sodium compound prepared by using fluid mechanics principle and preparation comprising cefoperazone sodium compound
  • Cefoperazone sodium compound prepared by using fluid mechanics principle and preparation comprising cefoperazone sodium compound
  • Cefoperazone sodium compound prepared by using fluid mechanics principle and preparation comprising cefoperazone sodium compound

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Experimental program
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Embodiment 1

[0035] Embodiment 1: the preparation of cefoperazone sodium compound

[0036] making process:

[0037]Measure 500ml of ethyl acetate and 100ml of water and add them to the standing wave reactor of the hydrodynamic principle device. While stirring, 25.01 g of sodium carbonate was slowly added. Adjust the pH value to 6.2. After the pH value is stable, add 0.21 g of activated carbon, decolorize for 30 min, and filter. Wash the carbon cake successively with acetone 50ml×2 and water 50ml×2. The temperature of the solvent circulation tank is controlled at 18-20°C, the temperature of the standing wave reactor is controlled at 30-35°C, the circulation pump is turned on, and 300ml of acetone is added dropwise to the standing wave reactor. Crystallize for 30min. Slowly lower the temperature of the solvent circulation tank to 8-10°C, turn on the circulation pump, continue to add 50ml of acetone dropwise, turn off the circulation pump, and stand for crystallization for 2 hours. Sucti...

Embodiment 2

[0039] Embodiment 2: the preparation of cefoperazone sodium compound

[0040] Measure 600ml of ethyl acetate and 100ml of water and add them to the standing wave reactor of the hydrodynamic principle device. While stirring, 25.02 g of sodium carbonate was slowly added. Adjust the pH value to 5.1, and after the pH value is stable, add 0.20 g of activated carbon, decolorize for 30 min, and filter. Wash the carbon cake successively with acetone 50ml×2 and water 50ml×2. The temperature of the solvent circulation tank is controlled at 15-18°C, the temperature of the standing wave reactor is controlled at 30-35°C, the circulation pump is turned on, and 300ml of acetone is added dropwise to the standing wave reactor. Crystallize for 30min. Slowly lower the temperature of the solvent circulation tank to 5-8°C, turn on the circulation pump, continue to add 50ml of acetone dropwise, turn off the circulation pump, and let it stand for crystallization for 2 hours. Suction filtration, ...

Embodiment 3

[0042] Embodiment 3: the preparation of cefoperazone sodium compound

[0043] Measure 400ml of ethyl acetate and 100ml of water and add them to the standing wave reactor of the hydrodynamic principle device. While stirring, 25.04 g of sodium carbonate was slowly added. Adjust the pH value to 6.5. After the pH value is stable, add 0.25 g of activated carbon, decolorize for 30 min, and filter. Wash the carbon cake successively with acetone 50ml×2 and water 50ml×2. The temperature of the solvent circulation tank is controlled at 10-15°C, the temperature of the standing wave reactor is controlled at 30-35°C, the circulation pump is turned on, and 300ml of acetone is added dropwise to the standing wave reactor. Crystallize for 30min. Slowly lower the temperature of the solvent circulation tank to 2-5°C, turn on the circulation pump, continue to add 50ml of acetone dropwise, turn off the circulation pump, and let it stand for crystallization for 2h. Suction filtration, and the f...

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PUM

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Abstract

The invention discloses a cefoperazone sodium compound prepared by using the fluid mechanics principle. Research&Development and Industrialization Project of High-end Medical Product Refinement Crystallization Technologies wins the second prize of national scientific and technological progress in 2015, and the fluid mechanics principle crystallization technology belongs to one of the high-end medical product refinement crystallization technologies. The cefoperazone sodium compound is determined by using X-ray powder diffraction, and the main characteristic peaks represented by the diffraction angle 2 theta in a map are located at 10.25+ / -0.2 degrees, 14.40+ / -0.2 degrees, 18.51+ / -0.2 degrees, 23.14+ / -0.2 degrees, 29.10+ / -0.2 degrees, 33.25+ / -0.2 degrees and 38.45+ / -0.2 degrees. Cefoperazone acid reacts with a salt forming agent, and the cefoperazone sodium compound is prepared through secondary crystallization. The operation is simple, reactants are easy to obtain, the reaction condition is mild, and the yield is high. The compound is high in purity, low in impurity content, good in fluidity and good in stability. Meanwhile, the invention further discloses a preparation prepared from cefoperazone sodium, namely, cefoperazone sodium for injection. The preparation process of the preparation is simple, no excipient is needed, and the preparation has better stability and few side effects.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a cefoperazone sodium compound prepared by utilizing the principle of fluid mechanics and a preparation thereof. 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 crystallization technology based on the principle of fluid mechanics is 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 achieve a leap in high-end pharmaceutical product research and development and crystallization technology. The international leading leve...

Claims

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Application Information

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IPC IPC(8): C07D501/36A61K31/546A61P31/00
CPCC07D501/36
Inventor 王坤
Owner 陕西顿斯制药有限公司
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