Preparation method of high-purity 3-deacetylcephalosporin C sodium salt

Abstract

The invention provides a preparation method of high-purity 3-deacetylcephalosporin C sodium salt. The preparation method comprises the following steps: (1) dissolving; (2) cracking; (3) crystallizing;and (4) filtering and drying. According to the preparation method, local peracid in the crystallization process can be avoided, degradation is reduced, the usage amount of concentrated hydrochloric acid and ammonia water is reduced, obvious economic benefits are achieved, meanwhile, erosion of chloride ions to production equipment is reduced, loss of the equipment is reduced, the volume of a mother liquor can be reduced, and the yield is increased. The purity of the 3-deacetylcephalosporin C sodium salt prepared by the preparation method disclosed by the invention is greater than 99% of DCPC;when the3-deacetylcephalosporin C sodium salt is used as a reference substance, the content of DCPC can be more accurately detected, the content of DCPC can be better controlled and reduced in CPC, DAOC and 7-ACA and 7-ADCA production, and the product quality is improved.

Description

technical field [0001] The invention relates to the technical field of pharmacy, in particular to a preparation method of high-purity 3-deacetylcephalosporin C sodium salt. Background technique [0002] In the antibiotic family, cephalosporin antibiotics are a relatively large branch, and they are also commonly used clinically for the treatment of bacterial infections. The source of cephalosporin antibiotics mainly depends on synthesis or semi-synthesis, generally with 7-aminocephalosporanic acid (abbreviated as 7-ACA) as the parent. Cephalosporin C (CPC for short) is an important intermediate for the production of 7-ACA. In the process of fermentation and production of CPC and DAOC, there is also a certain amount of 3-deacetylcephalosporin C sodium salt (DCPC), and DCPC eventually It will affect the product quality of 7-ACA or 7-ADCA. [0003] At present, the impurity DCPC is detected by the liquid phase area normalization method. The detection is affected by its low cont...

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Problems solved by technology

[0003] At present, the impurity DCPC is detected by the liquid phase area normalization method. The detection is affected by its low content, and the data is not accurate enough, which affects the quality of CPC sodium salt or DAOC.

It is an inevitable trend to prepare high-purity DCPC as a reference substance for the detection of impurity DCPC in CPC sodium salt or DAOC. However, in the prior art, DCPC is mainly obtained by separation and purification from fermentation waste liquid. This method has complicated process and low purity. Low yield, such as Yu Haijun. Isolation of deacetylcephalosporin C and synthesis of related compounds [D]. Tianjin: Tianjin University, 2006: 1-113.

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