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Method for refining ceftriaxone sodium crude product

A technology of ceftriaxone sodium and its refining method, which is applied in the field of chemical pharmacy, can solve problems such as instability of ceftriaxone sodium, high color grade of the product, and influence on the quality of ceftriaxone sodium, so as to improve safety and effectiveness, solvent Easy to get, cheap results

Active Publication Date: 2014-04-16
QILU ANTIBIOTICS PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Ceftriaxone sodium is prone to degradation reactions during the crystallization process, mainly because ceftriaxone sodium is unstable in a pure water system and is easily oxidized and degraded to produce degradation products, which cause high color grades of the product and directly affect the quality of ceftriaxone sodium

Method used

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  • Method for refining ceftriaxone sodium crude product

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Comparison scheme
Effect test

Embodiment 1

[0027] The refining method of embodiment 1, ceftriaxone sodium, the steps are as follows:

[0028] (1) Weigh 50 g of crude ceftriaxone sodium and 0.5 g of sodium metabisulfite, add a mixed solvent consisting of 10 ml of methanol and 60 ml of water, stir at room temperature for 30 min, add 1 g of activated carbon for decolorization for 20 min.

[0029] (2) The above solution is filtered through nitrogen pressure, and activated carbon and other impurities are removed by a microporous membrane. Then use the same proportion of water-methanol mixed solvent (5ml methanol and 30ml water) to wash the suction filter flask, wash the filter cake, and transfer to the crystallizer together.

[0030] (3) When the solution in the crystallizer reaches the crystallization temperature, start to add 50ml of fresh acetone dropwise. After the acetone is added dropwise, add sterile grade ceftriaxone sodium seed crystals. After growing the crystal for 30min, continue to add 370ml of acetone, and add...

Embodiment 2

[0033] The refining method of embodiment 2, ceftriaxone sodium, the steps are as follows:

[0034] (1) Weigh 50 g of crude ceftriaxone sodium and 1 g of sodium metabisulfite, add a mixed solvent consisting of 12 ml of methanol and 60 ml of water, stir at room temperature for 30 min, add 1 g of activated carbon for decolorization for 20 min.

[0035] (2) The above solution is filtered through nitrogen pressure, and activated carbon and other impurities are removed by a microporous membrane. Then use the same proportion of water-methanol mixed solvent (6ml methanol and 30ml water) to wash the suction filter flask, wash the filter cake, and transfer to the crystallizer together.

[0036] (3) When the solution in the crystallizer reaches the crystallization temperature, start to add 45ml of fresh acetone dropwise, add sterile grade ceftriaxone sodium seed crystals, continue to add 375ml of acetone after growing the crystal for 30min, add a total of 420ml of acetone, and crystalliz...

Embodiment 3

[0039] The refining method of embodiment 3, ceftriaxone sodium, the steps are as follows:

[0040] (1) Weigh 50 g of crude ceftriaxone sodium and 1 g of sodium metabisulfite, add a mixed solvent consisting of 14 ml of methanol and 60 ml of water, stir at room temperature for 30 min, add 1 g of activated carbon for decolorization for 20 min.

[0041] (2) The above solution was filtered by nitrogen pressure. Activated carbon and other impurities are removed by a microporous membrane. Then use the same proportion of water-methanol mixed solvent (7ml methanol and 30ml water) to wash the suction filter flask, wash the filter cake, and transfer to the crystallizer together.

[0042] (3) When the solution in the crystallizer reaches the crystallization temperature, start to drop 40ml of fresh acetone, add sterile grade ceftriaxone sodium seed crystals, continue to add 380ml of acetone after 30min of crystal growth, add a total of 420ml of acetone, and crystallize for 4.5 hours.

[...

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Abstract

The invention relates to a method for refining a ceftriaxone sodium crude product. The method comprises the following steps of: adding the ceftriaxone sodium crude product and sodium metabisulfite into a mixed solvent of water for injection and methanol, and dissolving until the solution is clarified; sterilizing the solution, filtering, and adding a leaching agent; adding ceftriaxone sodium seed crystals, and cultivating crystals after the crystals are precipitated; and continuing to add the leaching agent, precipitating the crystals completely, washing the crystals and drying to obtain a ceftriaxone sodium refined product. In the method, the mixed solvent is used as an initial solvent of the ceftriaxone sodium to improve the stability of the ceftriaxone sodium in a single hydrosolvent system; and in the presence of the sodium metabisulfite, the product is low in total impurities, less in degradation and stable in colors, the color of the ceftriaxone sodium refined product is No.1 lighter than that of crystals in the single hydrosolvent system, and the purity and quality of the product are improved.

Description

technical field [0001] The invention relates to the field of chemical pharmacy, in particular to a method for refining crude crystalline ceftriaxone sodium, which is used for preparing the refined ceftriaxone sodium. Background technique [0002] Molecular formula of ceftriaxone sodium: C 18 h 17 N 8 NaO 7 S 3 , the structural formula is as follows: [0003] [0004] The chemical name of ceftriaxone sodium is (6R,7R)-3-[[(1,2,5,6-tetrahydro-2-methyl-5,6-dioxo-1,2,4-triazine -3-yl)thio]methyl]-7-[[(2-amino-4-thiazolyl)methoxyiminoacetyl]amino]-8-oxo-5-thia-1-aza Sodium bicyclo[4.2.0]oct-2-ene-2-carboxylate. It is white or off-white crystalline powder, odorless and tasteless, hygroscopic, easily soluble in water, slightly soluble in methanol, almost insoluble in chloroform or ether. [0005] Ceftriaxone sodium was developed by Swiss Hoffmann-LaRoche Company and first launched in Switzerland in 1982. Belonging to the third generation of cephalosporin antibiotics, it...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/36C07D501/12
Inventor 侯传山王欣吴记勇杨燕冯宪东孙厚斌李玉斋
Owner QILU ANTIBIOTICS PHARMA
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