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Method for recycling active ingredients in amoxicillin mother liquor synthesized by enzymatic method

A technology for synthesizing amoxicillin mother liquor by enzymatic method, which is applied in the field of enzymatic synthesis of amoxicillin mother liquor by recycling macroporous resins, can solve the problems of unstable chemical properties, poor product purity, complex components, etc., and avoid adverse reactions , low equipment requirements, and simple process operation

Active Publication Date: 2012-12-12
NORTH CHINA PHARM GRP SEMISYNTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, in the hydrolysis mother liquor, it not only contains chemically unstable 6-APA, but also contains D-p-hydroxyphenylglycine and a large amount of impurities. Therefore, it is directly concentrated by nanofiltration membrane, which not only consumes a lot of energy, but also consumes a large amount of water in the concentrated solution. The composition is complex, so the isoelectric point method is used to separate 6-APA and D-p-hydroxyphenylglycine methyl ester, the efficiency is low, and the product purity is poor

Method used

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  • Method for recycling active ingredients in amoxicillin mother liquor synthesized by enzymatic method
  • Method for recycling active ingredients in amoxicillin mother liquor synthesized by enzymatic method

Examples

Experimental program
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Effect test

Embodiment 1

[0033] (a) Take 2000L of the mother liquor of amoxicillin synthesized by enzymatic method (among them, the content of residual amoxicillin is 3 mg / mL, the content of D-hydroxyphenylglycine is 15 mg / mL, and the content of D-hydroxyphenylglycine methyl ester is 5 mg / mL). Adjust the pH to 7.5 with sodium hydroxide solution, add 50kg of penicillin acylase, control the temperature at 25°C, and react for 2 hours to hydrolyze the amoxicillin in the mother liquor to generate D-hydroxyphenylglycine and 6-aminopenicillanic acid, D - hydrolysis of p-hydroxyphenylglycine methyl ester to D-p-hydroxyphenylglycine to obtain a hydrolyzate. The content of each component in the hydrolyzate was detected by high performance liquid chromatography, and the content of D-p-hydroxyphenylglycine was 18 mg / mL, and the content of 6-APA was 2 mg / mL.

[0034] (b) Use hydrochloric acid with a volume ratio of 15% to adjust the pH of the hydrolyzate to 6.0-7.0, and then separate the hydrolyzate through H103 ...

Embodiment 2

[0042] See the process flow figure 1 , the operation steps are as follows:

[0043] After enzymatically synthesizing amoxicillin, extract amoxicillin, and then recover the mother liquor:

[0044] (a) Mother liquor hydrolysis: Use concentrated ammonia to adjust the pH of the enzymatically synthesized amoxicillin mother liquor (2000L) to 7.5, add penicillin acylase (50kg), react at 30°C for 1 hour, remove the acylase by filtration, and obtain a hydrolyzate ; Under the pH value and temperature conditions, after 1h of reaction, the remaining amoxicillin in the mother liquor is fully hydrolyzed into 6-APA and D-p-hydroxyphenylglycine, and the remaining substrate D-p-hydroxyphenylglycine methyl ester in the synthesis reaction is also hydrolyzed It is D-p-hydroxyphenylglycine.

[0045] (b) Resin separation: Use hydrochloric acid with a volume ratio of 34% to adjust the pH value of the hydrolyzate to 7.0, and use XAD-4 macroporous resin column (produced by Rohn & hass company in the...

Embodiment 3

[0050] (a) Mother liquor hydrolysis: use 10% sodium hydroxide solution by mass ratio to adjust the pH of the enzymatically synthesized amoxicillin mother liquor to 8.0, add penicillin acylase, react at 25°C for 2 h, remove the acylase by filtration, Obtain a hydrolyzate; under the pH value and temperature conditions, after 2 hours of reaction, the residual amoxicillin in the mother liquor is fully hydrolyzed into 6-APA and D-p-hydroxyphenylglycine, and the remaining substrate D-p-hydroxyphenylglycine methyl Esters are also hydrolyzed to D-p-hydroxyphenylglycine.

[0051] (b) Resin separation: use hydrochloric acid with a volume fraction of 15-34% to adjust the pH value of the hydrolyzate to 6.5, and use the XAD1600N macroporous resin column produced by Rohn & hass company in the United States to separate, the sample loading temperature is 18°C, and the flow rate is 1.5BV / h,

[0052] Elute with deionized water, the elution temperature is 30°C, and the flow rate is 3 BV / h. Re...

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Abstract

The invention discloses a method for recycling active ingredients in the amoxicillin mother liquor synthesized by an enzymatic method. The method includes synthesizing the amoxicillin mother liquor by the enzymatic method; separating the amoxicillin mother liquor through a macro-porous resin column, eluting the separated amoxicillin mother liquor by deionized water, and collecting an eluant rich in D-4-Hydroxyphenylglycine and an eluant rich in 6-amino penicillanic acid (APA) respectively; filtering the eluant rich in D-4-Hydroxyphenylglycine with Daltonian ultrafiltration membranes with a cutoff molecular weight of 150 to 200; performing nanofiltration concentration on the Daltonian ultrafiltration membranes for the filtered liquor with the cutoff molecular weight of 150 to 200, and standing, crystallizing and filtering the concentrated liquor to obtain solids, and drying the solids to obtain the D-4-Hydroxyphenylglycine. According to the method, the technological design is reasonable, the operation is convenient, the recycling effect is good, and energy is saved and the environment is protected.

Description

technical field [0001] The invention relates to a process for recycling organic mother liquor, in particular to a method for synthesizing amoxicillin mother liquor by adopting macroporous resin recycling and utilizing enzymatic method. Background technique [0002] Amoxicillin, also known as amoxycillin or amoxycillin, is one of the most commonly used penicillin-like broad-spectrum β-lactam antibiotics. There are usually two methods for synthesizing amoxicillin: one is chemical synthesis, and the other is enzyme-catalyzed synthesis. Enzyme-catalyzed synthesis, referred to as enzymatic method, is catalyzed by immobilized penicillin acylase, from the mother nucleus 6-aminopenicillanic acid (hereinafter referred to as 6-APA) and D-hydroxyphenylglycine methyl ester in the water phase Stir the reaction. Compared with the chemical synthesis method, it can avoid the use of various organic solvents and reagents-, and the reaction conditions are mild (room temperature and neutral),...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P13/04C12P37/00C12P7/62C12P37/04C07C229/36C07C227/40C07C227/42C07D499/42C07D499/18
CPCY02P20/10
Inventor 左丽华严正人李宏魏鹏尹松涛
Owner NORTH CHINA PHARM GRP SEMISYNTECH CO LTD
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