Purification method of cefazolin acid

A technology of cefazolinic acid and purification method, applied in the field of medicine, can solve the problems of unstable purification process, complex synthesis route, long process and the like, and achieve the effects of less visible foreign matter, high yield and low impurity content

Active Publication Date: 2019-05-14
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] "A Method for Preparing Cefazolin Sodium Compound" (CN102321101B) and "A Method for Preparing Cefazolin Compound" (CN102617607B) mainly introduce the method of synthesizing cefazolin acid with 7-ACA as the mother nucleus, and the synthetic route is complicated , the process is too long
[0006] "A Purification Method for Cefazolin Acid" (CN104610282B)...

Method used

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  • Purification method of cefazolin acid
  • Purification method of cefazolin acid
  • Purification method of cefazolin acid

Examples

Experimental program
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Effect test

Embodiment 1

[0035] A method for purifying cefazolin, using cefazolin that does not meet quality requirements as raw material, comprising the steps of:

[0036] A. Take 20g of cefazolin acid, add 80ml of purified water, control the temperature at 20°C, add saturated sodium carbonate solution to adjust the pH of the system to 6.3, and stir until it dissolves;

[0037] B. Add 100mL ethyl acetate and stir for 10min, let stand for 10min to extract and separate phases, keep the water phase;

[0038] C. Add 5mL acetone and 5mL buffer solution to the water phase, control the temperature at 15°C, and add dropwise hydrochloric acid to adjust the pH of the system to 4.0, then add 0.1g of cefazolin acid seed crystals, and grow crystals for 30min at a time; wherein the buffer solution consists of It is prepared from citric acid and disodium hydrogen phosphate plus purified water. The mass volume of citric acid in the buffer solution is 11.8g / L, and the mass volume of disodium hydrogen phosphate is 27....

Embodiment 2

[0042] A method for purifying cefazolin, using cefazolin that does not meet quality requirements as raw material, comprising the steps of:

[0043] A. Take 20g of cefazolin acid, add 60mL of purified water, control the temperature at 25°C, add saturated sodium bicarbonate solution to adjust the pH of the system to 6.1, and stir until it dissolves;

[0044] B. Add 60mL of dichloromethane and stir for 10min, let it stand for 10min, extract and separate phases, and keep the water phase;

[0045] C. Add 10mL acetone and 5mL buffer solution to the water phase, control the temperature at 18°C, and add dropwise hydrochloric acid to adjust the pH of the system to 4.3, then add 0.02g cefazolin acid seed crystals, and grow crystals for 60min at a time; wherein the buffer solution consists of It is prepared from citric acid and disodium hydrogen phosphate plus purified water. The mass volume of citric acid in the buffer solution is 11.8g / L, and the mass volume of disodium hydrogen phosph...

Embodiment 3

[0049] A method for purifying cefazolin, using cefazolin that does not meet quality requirements as raw material, comprising the steps of:

[0050] A. Take 20g of cefazolin acid, add 70mL of purified water, control the temperature at 22°C, add saturated sodium carbonate solution to adjust the pH of the system to 6.2, and stir until it dissolves;

[0051] B. Add 80mL ethyl acetate and stir for 20min, let stand for 30min, extract and separate phases, keep the water phase;

[0052] C. Add 10mL acetone and 5mL buffer solution to the mixed solution, control the temperature at 17°C, and add dropwise hydrochloric acid to adjust the pH of the system to 4.18, then add 0.05g cefazolin acid seed crystals, and grow crystals for 45min at a time; wherein the buffer solution consists of It is prepared from citric acid and disodium hydrogen phosphate plus purified water. The mass volume ratio of citric acid in the buffer solution is 11.8g / L, and the mass volume ratio of disodium hydrogen phos...

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Abstract

The invention discloses a purification method of cefazolin acid, and belongs to the technical field of medicines. The purification method of the cefazolin acid comprises the following steps: A, addingraw materials into purified water, controlling the temperature, adding alkali liquor to adjust the pH of a system, and stirring until the solution is clear; B, adding an organic solvent and stirring,standing for phase separation, and retaining a water phase; C, adding acetone and a buffer solution into the water phase, controlling the temperature, dropwise adding an acid solution to regulate thepH value of the system, adding a seed crystal, and carrying out primary crystal growing; D, adding purified water, dropwise adding an acid solution to adjust pH, cooling and secondarily growing crystals; and E, filtering to obtain a filter cake, washing the filter cake at first, drying the filter cake under vacuum and discharging to obtain the purified cefazolin acid. The purified cefazolin acidobtained by the purification method not only meets the requirement of preparation of the cefazolin acid by a subsequent freeze-drying method, but also can be applied to preparation of high-content cefazolin acid standard substances.

Description

technical field [0001] The invention relates to cephalosporins, in particular to cefazolin acid, and belongs to the technical field of medicine. Background technique [0002] Cefazolin acid is used to synthesize cefazolin sodium, which is the first generation of 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. Cefazolin acid chemical name: (6R,7R)-3-[[(5-methyl-1,3,4-thiadiazol-2-yl)sulfur]met...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/12
Inventor 贾全田洪年胡利敏张锁庆李庆伟石春利任峰刘树斌魏宝军贺娇
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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