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Method for crystallizing cefoperazone sodium

A technology of cefoperazone sodium and cefoperazone acid is applied in the field of crystallization of cefoperazone sodium to achieve the effects of uniform crystal particle size distribution, accelerating crystallization process and preventing coalescence

Active Publication Date: 2010-10-20
FUJIAN FUKANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] At present, the dissolution and crystallization method is mainly used for production in China, but there is crystal coalescence in the production process, resulting in a small particle size of the final product and great difficulty in filtration , the product is mixed with a large amount of crystallization mother liquor, which affects the quality of the finished product
The method of adding seed crystals can effectively improve the crystal coalescence, but it has a certain impact on the particle size of the seed crystals and the particle size distribution of the crystals when the time is sufficient, resulting in fluctuations in the quality of the finished product

Method used

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  • Method for crystallizing cefoperazone sodium
  • Method for crystallizing cefoperazone sodium

Examples

Experimental program
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Embodiment 1

[0023] Add 65ml of acetone to a 250ml three-necked bottle, add 32g of cefoperazone acid under stirring, cool down to 8~10℃, add NaHCO dropwise 3 Adjust the pH of the saturated solution to 6.2~6.8, and maintain this pH until the solid dissolves completely, filter, move the filtrate to a 1000ml three-necked bottle and place it in an ultrasonic generator, control the temperature of 13~18°C, add dropwise to the three-necked bottle while stirring Acetone 100ml, start the ultrasonic generator to seed the crystal for 30~40 minutes after dripping, continue to stir for 30 minutes, continue to drop acetone 700ml into the three-necked bottle, control the temperature at about 15℃, stir and grow the crystal for 70 minutes, filter, and use acetone 100ml of the filter cake was washed and drained, then vacuum-dried at 40°C until the moisture content was acceptable to obtain 30.5g of cefoperazone sodium, with a weight yield of 95.3%, clarity <0.5, sum of impurities: 0.10%, cefoperazone poly...

Embodiment 2

[0025] Add 50ml of acetone and 16ml of ethanol to a 250ml three-necked bottle, add 32g of cefoperazone acid under stirring, cool down to 8~10℃, add NaHCO dropwise 3 Adjust the pH of the saturated solution to 6.2~6.8, and maintain this pH until the solid dissolves completely, filter, move the filtrate to a 1000ml three-necked bottle and place it in an ultrasonic generator, control the temperature of 13~18°C, add dropwise to the three-necked bottle while stirring Acetone 90ml, start the ultrasonic generator to seed the crystal for 30~40 minutes after dripping, continue to stir for 30 minutes, continue to drop acetone 700ml into the three-neck bottle, control the temperature at about 15℃, stir and grow the crystal for 80 minutes, filter, and use acetone 100ml of the filter cake was washed and then sucked dry, vacuum-dried at 40°C until the moisture content was acceptable, and 30.0g of cefoperazone sodium was obtained, with a weight yield of 93.8%, the sum of impurities: 0.12%,...

Embodiment 3

[0027] Add 50ml of acetone and 16ml of isopropanol to a 250ml three-necked bottle, add 32g of cefoperazone acid under stirring, cool down to 8~10℃, add NaHCO dropwise 3 Adjust the pH of the saturated solution to 6.2~6.8, and maintain this pH until the solid dissolves completely, filter, move the filtrate to a 1000ml three-necked bottle and place it in an ultrasonic generator, control 13~18°C, and drop it into the three-necked bottle while stirring Add 90ml of acetone, turn on the ultrasonic generator to seed the crystal for 30~40 minutes after dripping, continue to stir for 30 minutes, continue to drop 700ml of acetone into the three-necked bottle, control the temperature at about 15°C, stir and grow the crystal for 80 minutes, filter, and use Wash the filter cake with 100ml of acetone and drain it, vacuum-dry at 40°C until the water content is acceptable, and obtain 29.6g of cefoperazone sodium, with a weight yield of 92.5%, the sum of impurities: 0.21%, cefoperazone polym...

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Abstract

The invention aims to provide a method for crystallizing cefoperazone sodium, which comprises the following steps of: dissolving cefobid in a solvent, and adding a salt forming agent to adjust the pH to between 6.2 and 6.8 until the solid is completely dissolved; and filtering, adding the filtrate into the solvent under the ultrasonic condition to separate out crystals, filtering, washing and leaching the crystals, and performing vacuum drying to obtain the cefoperazone sodium. Aiming at the problems in the industrial crystallization of the cefoperazone sodium, the ultrasonic radiation has strong orienting effect, supplements and enhances the wave action required by the formation of critical crystal nucleus, can accelerate graining process and promote the quick generation of the crystal nucleus, and achieves the effect of quickly graining without seeding by seed crystals; meanwhile, the ultrasonic in the liquid medium can make mass points in the medium obtain high acceleration, has the effect of cavitation, and can prevent the accumulation during crystal growth to make the size distribution of the crystals uniform.

Description

technical field [0001] The invention relates to a crystallization method of cefoperazone sodium, which belongs to the field of medicines. Background technique [0002] The chemical name of cefoperazone sodium is 7-[D(-)-X-(4-ethyl-2,3-dioxo-1-piperic acid amido)-X-(4-hydroxyphenyl)acetamido] -Sodium 3-[(1-methyl-1H-tetrazol-5-yl)thiomethyl]-3-cephem-4-carboxylate. The common name is also known as Pioneer mustsu, Pioneerone, etc., and the English name is Cefobine, Cefobis. The molecular structure is shown in Figure (1). [0003] [0004] figure 1) [0005] Cefoperazone sodium is used as an injection drug, and its clarity is a crucial indicator for examining the quality. The problem of clarity is a common problem faced by cephalosporins, and it is also a difficulty. [0006] From the structural formula of cefoperazone acid (2) [0007] [0008] figure 2) [0009] It can be seen that its molecule contains a β-lactam ring, which is not very stable under alkaline cond...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/36C07D501/12
Inventor 陈德福
Owner FUJIAN FUKANG PHARMA
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