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Process for purifying cefsulodin sodium by solvent crystallization method

A technology of cefsulodin sodium and sporoxalin, which is applied in the field of pharmacy, can solve the problems of high column chromatography cost, cumbersome operation, and low feasibility, and achieve the effects of stable product quality, simple operation, and reduced production cost

Active Publication Date: 2011-02-16
福安药业集团重庆博圣制药有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method is cumbersome to operate, and the cost of column chromatography is too high in industrial production, and the feasibility is very small; and the inventors have found that the ratio of ethanol-water in the mixed solvent is different, and the quality of the obtained product is very different. , but there is no report on this aspect in the current literature

Method used

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  • Process for purifying cefsulodin sodium by solvent crystallization method

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Experimental program
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Effect test

Embodiment 1

[0053] Dissolve 15.8g of sodium bicarbonate in 800ml of water, add 100g of cefsulodin at 0-5°C, the pH of the solution is 4.2-4.8, stir to dissolve, add 2.0g of activated carbon, decolorize for 0.5h, and filter. Control the temperature at 0-5°C, add 2500ml of ethanol and a small amount of seed crystals, and grow the crystals for 1 hour. Add 4000 ml of ethanol dropwise within 2 hours, grow the crystal for 1 hour, filter, and dry the filter cake in vacuum at 35°C for 3 hours to obtain 99.5 g of cefsulodin sodium with a yield of 95.4%, HPLC content of 99.7%, and related substances of 0.36%. (Conditions for HPLC determination of content: chromatographic column: Sephadex G-10 post, column temperature: 25°C, mobile phase: 0.05mol / L phosphate buffer (pH7.0), flow rate: 0.5ml / min , detection wavelength: 254nm, injection volume: 20μl, the same below)

Embodiment 2

[0055] Dissolve 10.0g of sodium carbonate in 600ml of water, control the temperature at 0-5°C, add 100g of cefsulodymic acid, the pH of the solution is 4.3-4.6, stir to dissolve, add 2.0g of activated carbon, decolorize for 0.5h, and filter. Control the temperature at 0-5°C, add 2,200ml of ethanol and a small amount of seed crystals, grow the crystals for 1 hour, add 3,800ml of ethanol dropwise within 2 hours, grow the crystals for 1 hour, filter, and dry the filter cake in vacuum at 35°C for 3 hours to obtain 100.4g of cefsulodin sodium. The yield is 96.3%, the HPLC content is 99.9%, and the related substances are 0.33%.

Embodiment 3

[0057] Dissolve 7.5g of sodium hydroxide in 600ml of water, control the temperature at 0-5°C, add 100g of cefsulodin, the pH of the solution is 4.2-4.5, stir to dissolve, add 2.0g of activated carbon, decolorize for 0.5h, and filter. Control the temperature of the filtrate at 0-5°C, add 2200ml of ethanol and a small amount of seed crystals, and grow the crystals for 1 hour. Add 3800ml of ethanol dropwise within 2 hours, grow crystals for 1 hour, filter, and dry the filter cake in vacuum at 35°C for 3 hours to obtain 99.8 g of cefsulodin sodium with a yield of 95.7%, HPLC content of 99.6%, and related substances of 0.32%.

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Abstract

The invention discloses a process for purifying cefsulodin sodium by a solvent crystallization method, which comprises the following steps: adding water, ethanol and a small amount of seed crystals into cefsulodin sodium, then carrying out crystal growing for 2 hours; filtering the obtained mixture, and then carrying out vacuum drying on the obtained mixture at a temperature of 35 DEG C so as to obtain refined cefsulodin sodium, wherein the HPLC content therein is 99.4 to 99.9 percent, and the volume ratio of water to ethanol is 1:(3 to 15). The process of the invention has the advantages of high required product content, low relevant material content, and good stability and reconstitution of the obtained product.

Description

technical field [0001] The invention relates to the technical field of pharmacy, in particular to a process for purifying cefsulodin sodium by solvent crystallization. technical background [0002] The chemical name of cefsulodin sodium is (6R,7R)-3-[(4-carbamoylpyridin-1-ium-1-yl)methyl]-8-oxo-7-[[(2R)- Sodium 2-phenyl-2-sulfoacetyl]amino]-5-thio-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylate, molecular formula C 22 h 19 N 4 NaO 8 S 2 , CAS RN: 52152-93-9, its structural formula is as follows: [0003] [0004] Cefsulodin sodium, developed by Takeda Corporation of Japan, is a narrow-spectrum, semi-synthetic third-generation cephalosporin antibiotic. Clinically dedicated to Pseudomonas aeruginosa infection, its antibacterial effect is almost the same as that of aminoglycoside antibiotics such as gentamicin and dideoxykanamycin, and has no cross-resistance with them; it is stronger than carbenicillin 16-32 times, about 10 times stronger than sulbenicillin. It was first...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/04C07D501/44C07D501/12
Inventor 蒋晨郭子维张稳稳
Owner 福安药业集团重庆博圣制药有限公司
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