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7-ACA with low content of maximum unknown single impurity and preparation method thereof

A low-content, maximum technology, applied in the field of biomedicine, can solve the problem of inability to effectively reduce the unknown single-impurity content of 7-ACA, and achieve the effect of simple operation and high production yield

Active Publication Date: 2021-04-09
YILI CHUANNING BIOTECH CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] One object of the present invention is to provide a kind of preparation method that is simple to operate, suitable for large-scale industrial production, and can reduce the maximum unknown simplex content in 7-ACA. Another object of the present invention is to provide the maximum 7-ACA with unknown simple impurities, solving the problem that existing processes (especially industrialized large-scale production processes) cannot effectively reduce the content of unknown simple impurities in 7-ACA

Method used

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  • 7-ACA with low content of maximum unknown single impurity and preparation method thereof
  • 7-ACA with low content of maximum unknown single impurity and preparation method thereof
  • 7-ACA with low content of maximum unknown single impurity and preparation method thereof

Examples

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Effect test

Embodiment 1

[0047] Example 1 The present invention prepares the method for 7-ACA with low content maximum unknown single heterogeneity

[0048] Specifically include the following steps:

[0049] (1) Take a cephalosporin C preparation solution with a potency of 21500 μg / mL and a pH of 7.0, add 0.2wt.‰ of sodium bisulfite, and mix well to obtain a pretreatment solution;

[0050] (2) react the pretreatment liquid obtained in step (1) with immobilized cephalosporin C acylase, control the reaction temperature at 14°C, the reaction pH is 8.3, and the reaction time is 80 minutes, and 7-ACA is obtained after the reaction ends Acylation solution;

[0051] (3) After the acylation solution collected in step (2) is ultrafiltered by an ultrafiltration membrane, the pH value is adjusted to 5.3 with 10% hydrochloric acid, and the isoelectric point crystallization is carried out to obtain 7-ACA crystals, which are then filtered and dried. That is, the finished product of 7-ACA is obtained.

Embodiment 2

[0052] Example 2 The present invention prepares the method for 7-ACA with low content maximum unknown single heterogeneity

[0053] Specifically include the following steps:

[0054] (1) Take the cephalosporin C preparation solution with a potency of 22000 μg / mL and a pH of 7.5, add 0.3wt.‰ of sodium bisulfite, and mix well to obtain a pretreatment solution;

[0055] (2) react the pretreatment liquid obtained in step (1) with immobilized cephalosporin C acylase, control the reaction temperature at 14°C, the reaction pH is 8.3, and the reaction time is 80 minutes, and 7-ACA is obtained after the reaction ends Acylation solution;

[0056] (3) After the acylation solution collected in step (2) is ultrafiltered by an ultrafiltration membrane, the pH value is adjusted to 5.3 with 10% hydrochloric acid, and the isoelectric point crystallization is carried out to obtain 7-ACA crystals, which are then filtered and dried. That is, the finished product of 7-ACA is obtained.

Embodiment 3

[0057] Example 3 The present invention prepares the method for 7-ACA with low content maximum unknown single heterogeneity

[0058] Specifically include the following steps:

[0059] (1) Take a cephalosporin C preparation solution with a potency of 22500 μg / mL and a pH of 7.3, add 0.23wt.‰ of sodium bisulfite, and mix well to obtain a pretreatment solution;

[0060] (2) react the pretreatment liquid obtained in step (1) with immobilized cephalosporin C acylase, control the reaction temperature at 14°C, the reaction pH is 8.3, and the reaction time is 80 minutes, and 7-ACA is obtained after the reaction ends Acylation solution;

[0061] (3) After the acylation solution collected in step (2) is ultrafiltered by an ultrafiltration membrane, the pH value is adjusted to 5.3 with 10% hydrochloric acid, and the isoelectric point crystallization is carried out to obtain 7-ACA crystals, which are then filtered and dried. That is, the finished product of 7-ACA is obtained.

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Abstract

The invention discloses 7-ACA with low content of maximum unknown single impurity and a preparation method of the 7-ACA, wherein the purity of the 7-ACA is 99.10% or more, and the maximum unknown single impurity content is 0.152% or less; the preparation method comprises the following steps: (1) adding the antioxidant into a cephalosporin C preparation solution, and uniformly mixing to obtain a pretreatment solution; (2) carrying out an enzymatic hydrolysis reaction on the pretreatment liquid obtained in the step (1) and an enzyme to obtain a 7-ACA enzymatic hydrolysate; and (3) carrying out ultrafiltration, crystallization and filtration on the enzymatic hydrolysate obtained in the step (2), and drying the solid to obtain the 7-ACA. By adding the antioxidant into the cephalosporin C preparation solution, the generation of the maximum unknown single impurity in the enzymolysis reaction process can be effectively reduced, and the content of the maximum unknown single impurity in the final product 7-ACA is effectively reduced; the method disclosed by the invention is simple to operate and suitable for industrial mass production, overcomes the technical problem that 7-ACA with low unknown single impurity content and high purity is difficult to prepare in industrial mass production in the prior art, and has a wide application prospect.

Description

technical field [0001] The invention belongs to the technical field of biomedicine, and in particular relates to a 7-ACA with a low content of the maximum unknown simplex and a preparation method thereof. Background technique [0002] 7-ACA (7-aminocephalosporanic acid) is a white or off-white crystalline powder, which is an important mother nucleus for the synthesis of cephalosporin antibiotics; it contains two active groups: 3-position acetoxy and The amino group at position 7 can form a variety of cephalosporin antibiotics with different properties by connecting different side chains on these two active groups, including cefazolin sodium, cefotaxime sodium, ceftriaxone sodium, cephalosporin sodium Piperton Sodium, Ceftazidime Sodium, Cefuroxime Sodium, etc. Cephalosporin antibiotics have been widely used because of their broad antibacterial spectrum, strong antibacterial effect, less allergic reactions, only partial cross-allergy with penicillin, and different degrees of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/18C07D501/12C12P35/02
CPCC07D501/12C07D501/18C12P35/02Y02P20/10
Inventor 朱洪生高旋阮卫国苏彦波杨勇王树林何强王瑞杨伟汤安刘建
Owner YILI CHUANNING BIOTECH CO