A kind of preparation method of high-purity cefazolin sodium and pharmaceutical preparation thereof

A technology of cefazolin sodium and cefazolin acid, which is applied in the directions of drug delivery, pharmaceutical formulations, antibacterial drugs, etc., can solve the problems of complicated operation, difficult removal of impurities in products, and high quality requirements of cefazolin acid, and achieves Simple operation, stable product quality and good process reproducibility

Active Publication Date: 2021-07-13
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] "A Method for Preparing Cefazolin Sodium Compound" (CN102321101B) mainly introduces that cefazolin acid sodium is directly freeze-dried, but the quality requirements for cefazolin acid are relatively high, and impurities in the product are difficult to remove
[0005] "A kind of purification method of cefazolin sodium" (CN110483554A) mainly introduces a kind of purification method of cefazolin sodium, but it uses dichloromethane phase separation, complicated operation, and a large amount of waste liquid is produced by adjusting pH with sodium hydroxide solution

Method used

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Examples

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preparation example Construction

[0031] The invention discloses a preparation method of high-purity cefazolin sodium and a pharmaceutical preparation thereof, comprising the following steps:

[0032] 1) Put a certain amount of cefazolin acid into a phosphate solution whose weight is 3 to 4 times that of cefazolin acid, stir evenly, and control the temperature at 28 to 32°C;

[0033] 2) Sodium carbonate with 12% of the weight of cefazolin acid is dropped into purified water with 4.2 to 12.5 times the weight of sodium carbonate, and the temperature is controlled at 30-40° C., stirring to dissolve;

[0034] 3) Sodium carbonate solution is slowly added to the mixed solution of cefazolin acid, phosphate solution and purified water, the phosphate is one of disodium hydrogen phosphate, sodium dihydrogen phosphate, potassium dihydrogen phosphate and dipotassium hydrogen phosphate, Concentration is 1mol / L, control temperature is 28~32 ℃, pH is 3.5~5.8, make cefazolin acid dissolve clear, add the aluminum oxide adsorbe...

Embodiment 1

[0040] Add 400 g of cefazolin acid into 100 mL of disodium hydrogen phosphate solution and 1200 mL of purified water, and stir at 28°C for 10 min. Put 48g of sodium carbonate into 200mL of water, control the temperature at 30°C, and stir to dissolve. Add the sodium carbonate solution to the cefazolin acid feed solution for 2 hours, keep at 28°C, adjust the pH to 3.5, and stir for 10 minutes. Add 20 g of alumina, stir for 1 hour and then filter, adjust the pH to 5.70 with lye, and then adjust the pH to 5.40 with phosphoric acid. After the feed solution was dissolved, 0.4 g of disodium edetate was added and stirred for 10 minutes. Slowly add 135 g of solid sodium chloride over 20 minutes and stir for 40 minutes; add 135 g of solid sodium chloride again for 1 hour. The temperature was lowered to -2°C to grow the crystal for 1 hour. Filter, and wash the filter cake twice with 300 mL of acetone. After drying at 40°C for 12 hours, the water content was less than 12.3%, and the y...

Embodiment 2

[0043]Add 400 g of cefazolin acid into 100 mL of sodium dihydrogen phosphate solution and 1600 mL of purified water, and beat at 32°C for 10 minutes. Put 48g of sodium carbonate into 600mL of water, control the temperature at 40°C during the process, and stir to dissolve. Add the sodium carbonate solution to the cefazolin acid feed solution for 1.5 hours, keep at 32°C, adjust the pH to 5.8, and stir for 10 minutes. Add 20 g of alumina, stir for 1 hour, filter, and adjust the pH to 5.45 with hydrochloric acid. After the feed solution was dissolved, 1.2 g of disodium edetate was added and stirred for 10 min. Slowly add 230 g of solid sodium chloride over 45 minutes and stir for 45 minutes; add 230 g of solid sodium chloride again for 1.5 hours. The temperature was lowered to 2°C for 5 hours to grow the crystal. Filter, and wash the filter cake twice with 500 mL of acetone. Dry at 55°C for 4 hours, the moisture is less than 11.5%, and the yield is 107.2%.

[0044] The cefazo...

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Abstract

The invention relates to a preparation method of high-purity cefazolin sodium and a pharmaceutical preparation thereof, belonging to the technical field of cefazolin sodium preparation, comprising the following steps: 1) putting cefazolin acid into a phosphate solution and stirring evenly , control the temperature; 2) Put the sodium carbonate into the purified water, control the temperature, and stir to dissolve; 3) Slowly add the sodium carbonate solution to the mixture of cefazolin acid, phosphate solution and purified water, control the temperature, pH, Dissolve cefazolin acid, add adsorbent to stir and filter, and adjust pH; 4) Add disodium edetate and sodium chloride solid, cool down and grow crystals; 5) Filter cefazolin sodium crystal solution, and use solvent Dip washing and drying. The invention can effectively remove various impurities and polymers in the cefazolin acid, and the obtained product has high purity and good quality, and has higher medicinal safety after being made into a powder injection.

Description

technical field [0001] The invention relates to a preparation method of high-purity cefazolin sodium and a pharmaceutical preparation thereof, belonging to the technical field of cefazolin sodium preparation. Background technique [0002] Cefazolin sodium is the first generation cephalosporin for injection. The antibacterial effect on positive cocci exceeds that of the second and third generations. Cefazolin sodium is unstable to the β-lactamase produced by negative bacilli, and some negative bacilli have been drug-resistant. It has no antibacterial activity against Pseudomonas aeruginosa, Enterobacter bacilli and anaerobic Bacteroides fragilis. It can be used for respiratory tract, genitourinary tract, biliary tract, skin and soft tissue infection caused by sensitive pathogenic bacteria, postoperative infection, trauma infection, eye, ear, nose and throat infection and surgical perioperative prophylaxis. The chemical name of cefazolin sodium is: (6R,7R)-3-[[(5-methyl-1,3...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/36A61K31/546A61P31/04A61K9/14
CPCA61K9/0019A61K9/14A61K31/546A61P31/04C07D501/36
Inventor 贾全刘树斌张建丽张锁庆任峰田洪年魏宝军杨梦德贺娇
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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