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Process for preparing 7-ADCA by taking DAOC fermentation liquor as raw material

A 7-ADCA and fermented liquid technology, applied in fermentation, organic chemistry, etc., can solve the problems of complicated process, low product purity and yield, low purity, etc., and achieve the effect of simple operation process, high conversion rate and simplified process

Pending Publication Date: 2021-10-22
AMICOGEN CHINA BIOPHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its patent No. CN1357051A of Leon Company of Spain discloses a production process of utilizing biological method to prepare 7-ADCA, and introduces the process of using DAOC as substrate to produce 7-ADCA, but in the preparation process, DAOC needs to be concentrated first, and then , using organic solvents for crystallization to obtain low-purity DAOC crystals, and then using two-step enzymatic methods combined with strong oxidants for cracking, and finally using organic matter for separation and purification. Although this process simplifies the original production process, but in production, The process is still relatively complicated, and organic solvents and strong oxidants are still needed, and the purity and yield of the product are relatively low

Method used

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  • Process for preparing 7-ADCA by taking DAOC fermentation liquor as raw material
  • Process for preparing 7-ADCA by taking DAOC fermentation liquor as raw material
  • Process for preparing 7-ADCA by taking DAOC fermentation liquor as raw material

Examples

Experimental program
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Effect test

Embodiment 1

[0054] (1) After the fermentation, take 1.5L of DAOC fermentation broth, add 4mol / L sodium hydroxide solution, adjust the pH of the fermentation broth to 11, and centrifuge at 8000 to remove large insoluble particles, and wash the centrifuged solids with a certain amount of water. Obtain the mixed feed liquid of supernatant liquid and cleaning liquid, adjust feed liquid pH=3.5, place for subsequent use;

[0055] (2) Use macroporous adsorption resin for preliminary extraction of the treatment solution: the resin is DM1180 macroporous adsorption resin produced by Amicogen (China) Biomedical Co., Ltd. (40mL, specific surface is 450㎡ / g, pore diameter is 16nm, ) is the pre-column, DM700 resin (500mL, specific surface is 1360㎡ / g, pore size is 6nm,) is the adsorption column, the upper column liquid is the pretreatment liquid, the upper column volume is 1.3L (25.74g), and the adsorption flow rate is 1.0BV / h, wash 4BV of water, the flow rate is 1BV / h, the adsorption capacity is 51.28m...

Embodiment 2

[0061] (1) After the fermentation, take 1.5L of DAOC fermentation broth, add 4mol / L sodium hydroxide solution, adjust the pH of the fermentation broth to 9.5, and centrifuge at a speed of 10,000 to remove large insoluble particles, and wash the centrifuged solids with a certain amount of water. Obtain the mixed feed liquid of supernatant liquid and cleaning liquid, adjust feed liquid pH=4.0, place for subsequent use;

[0062] (2) Use macroporous adsorption resin for preliminary extraction of the treatment solution: the resin is DM1180 macroporous adsorption resin produced by Amicogen (China) Biomedical Co., Ltd. (45mL, specific surface is 450㎡ / g, pore diameter is 12nm) It is a pre-column, DM700 resin is (520mL, specific surface is 1280㎡ / g, pore size is 8nm), adsorption column, the upper column liquid is pretreatment liquid, the upper column volume is 1.4L (27.72g), and the adsorption flow rate is 1.5BV / h , washed with 6BV of water, the flow rate is 1BV / h, the adsorption capaci...

Embodiment 3

[0068] (1) After the fermentation, take 1.5L of DAOC fermentation broth, add 4mol / L sodium hydroxide solution, adjust the pH of the fermentation broth to 10.8, and centrifuge at 10,000 to remove large insoluble particles, and wash the centrifuged solids with a certain amount of water. Obtain the mixed feed liquid of supernatant liquid and cleaning liquid, adjust feed liquid pH=3.0, place for subsequent use;

[0069] (2) Use macroporous adsorption resin for preliminary extraction of the treatment solution: the resin is DM1180 macroporous adsorption resin (40mL, specific surface: 350㎡ / g, pore diameter: 14nm) produced by Amicogen (China) Biomedical Co., Ltd. Pre-column, DM700 resin is (480mL, specific surface is 1200㎡ / g, pore size is 7nm), adsorption column, the upper column liquid is the pretreatment liquid, the upper column volume is 1.1L (20.92g), the adsorption flow rate is 3BV / h, wash with water 6BV of water, the flow rate is 3BV / h, the adsorption capacity is 39.42mg / mL, the...

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Abstract

The invention relates to a method for separation and purification of DAOC and preparation of 7-ADCA. The method comprises the following steps: (1) pretreatment of DAOC fermentation liquor: firstly, adjusting the pH value of the fermentation liquor, and conducting filtering via a filter screen to remove insoluble large-particle impurities; (2) primary extraction of treatment liquor via two macroporous adsorption resin tandem columns; (3) decoloration treatment of desorption liquid via anion exchange resin; (4) conversion into 7-ADCA via one-step acylase lysis; (5) decolorization with activated carbon; and (6) pH value adjustment and crystallizing. According to the invention, the use amount of an organic solvent can be reduced, and environment protection is facilitated. According to the invention, the production of pollutants can be reduced in virtue of regeneration and recycling of the resin, the process is simple to operate, the disadvantages of conventionally used strong oxidant are changed, high safety is obtained, the extraction rate of the DAOC fermentation liquor is high and can achieve 95% or more, the total yield of a 7-ADCA product is 46-48%, the purity of the obtained 7-ADCA product is high and can achieve 99.5 or more, and the content of 7-ADCA can achieve 99% or more.

Description

technical field [0001] The invention belongs to the technical field of separation and extraction of biologically active components and preparation of a compound, and more specifically relates to a method for extracting and separating DAOC from biological fermentation liquid and preparing the compound 7-ADCA. Background technique [0002] 7-aminodeacetoxycephalosporanic acid (7-ADCA) is the main starting material for the synthesis of semi-synthetic antibiotics cephalosporins, such as cefadroxil, cephalexin and cephradine. Its molecular structure is as follows: [0003] [0004] 7-Aminodeacetoxycephalosporanic acid (7-ADCA) is a substrate used in the preparation of specific cephalosporins with functional deletions at position 3. At present, its domestic preparation method is mainly chemical method, patent CN101735246 and literature (Liu Dongzhi, Qu Hongmei, Zhang Tianyong. Synthesis progress of 7-ADCA [J] Foreign Medicine and Antibiotics Volume, 1998, 19(4): 267-268 .) di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/22C07D501/12C12P35/02
CPCC07D501/22C07D501/12C12P35/02
Inventor 律恩法贾延宝王玲赵新祥何海潮
Owner AMICOGEN CHINA BIOPHARM CO LTD
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