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Preparation method of high-purity cefazolin sodium and medicinal 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, mild acid-base reaction process, good process reproducibility

Active Publication Date: 2020-08-18
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • 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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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 medicinal preparation thereof, which belongs to the technical field of cefazolin sodium preparation, and the methodcomprises the following steps: 1) adding cefazolin acid into a phosphate solution, uniformly stirring, and controlling the temperature; 2) adding sodium carbonate into purified water, controlling thetemperature, stirring and dissolving; 3) slowly adding a sodium carbonate solution into the mixed solution of cefazolin acid, a phosphate solution and purified water, controlling the temperature and pH to dissolve the cefazolin acid to be clear, adding an adsorbent, stirring and filtering, and adjusting the pH; (4) adding ethylenediamine tetraacetic acid disodium and sodium chloride solid, coolingand growing crystals; and (5) filtering a cefazolin sodium crystallization solution, leaching and washing with a solvent, and drying. According to the invention, the method can effectively remove various impurities and polymers in cefazolin acid, the obtained product is high in purity and quality, and the prepared powder injection has higher medicinal safety.

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 Applications(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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