Method for extracting crystallized erythromycin thiocyanate from fermentation liquid

A technology of erythromycin thiocyanate and fermentation broth, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., to achieve the effects of avoiding damage, reducing impurity content, and high-efficiency filtration

Active Publication Date: 2013-11-27
NINGXIA QIYUAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to solve the problems mentioned above brought by the extraction process of microfiltration membrane+resin or plate frame+extraction in the prior art, and to provide a method for separating and crystallizing erythromycin thiocyanate from erythromycin fermented liquid method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take 50L of erythromycin fermentation broth, and filter it with an organic plate membrane with a pore size of 5-50nm under the conditions of pH 8.0 and pressure 0.2MPa. During the process, a peristaltic pump flow is added to pure water for dialysis; the obtained filtrate 110L is subjected to roll-type nanofiltration Membrane concentration, the membrane with a molecular weight cut-off of 700 or more, the pH of the filtrate during the concentration process is controlled at 6.5~7.5, the pressure is controlled at 4.0MPa, and the concentration of the obtained concentrate is 2.23g / 100ml; the concentrate is fed with 15% thiocyanate solution to crystallize. Get 100g of erythromycin crystalline coarse salt and dissolve in 500ml of amyl acetate, adjust pH 11.8, the concentration of lysate red A is 12.48%, and the polarity of mixed solvent is 4.8, separate to obtain the upper layer of amyl acetate solution, add 1% activated carbon to filter, and add to Add 1000ml of acetone to this...

Embodiment 2

[0028] Take 50L of erythromycin fermentation liquid, under the conditions of pH 8.2 and pressure 0.22MPa, use an organic plate membrane with a pore size of 5-50nm to filter. During the process, a peristaltic pump flow is added to pure water for dialysis, and 110L of the obtained filtrate is concentrated by nanofiltration. For a membrane with a molecular weight cut-off of 700 or more, the pH of the filtrate during the concentration process is controlled at 6.5~7.5, the pressure is controlled at 3.9MPa, and the concentration of the obtained concentrated solution is 2.12g / 100ml; the concentrated solution is fed with 10% ammonia water. Dissolve 100g of erythromycin crude base in 500ml of butyl acetate, adjust the pH to 11.8, the concentration of erythromycin A in the solution is 11.4%, separate and obtain the upper layer of butyl acetate solution, add 1.5% activated carbon to filter, and add 1500ml of acetone, the volume percentage of acetone in the solution is 75.0%, the polarity ...

Embodiment 3

[0031] Take 70L of erythromycin fermentation broth, under the conditions of pH 7.8 and pressure 0.16MPa, use an organic plate membrane with a pore size of 5-50nm to filter. During the process, a peristaltic pump flow is added to pure water for dialysis, and 160L of the obtained filtrate is concentrated by nanofiltration. The nanofiltration membrane is a membrane with a molecular weight cut-off of 700 or more. During the concentration process, the pH of the filtrate is controlled at 6.5~7.5, the pressure is controlled at 3.8MPa, and the concentration of the obtained concentrated solution is 2.22g / 100ml; the concentrated solution is fed with 15% thiocyanate solution. Take 160g of crude erythromycin thiocyanate and dissolve it in 500ml of dichloromethane, adjust the pH to 11.8, the concentration of the solution red A is 20.3%, separate and obtain the lower layer of dichloromethane solution, add 1.5% activated carbon to filter, and add 2000ml of acetone, the volume percentage of ac...

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Abstract

The invention relates to a method for extracting crystallized erythromycin thiocyanate by separating macrolide antibiotic from an erythromycin fermentation liquid, and belongs to the field of erythromycin separation crystallization. The separation and extraction method comprises the steps that an ultrafiltration membrane is used for filtration; a filtrate is subjected to nano filtration concentration; erythromycin in a concentrated solution is transferred to a preliminary solvent under an alkaline condition; an aqueous phase is separated and removed; and a main solvent is added after the solution is subjected to decoloration and filtration; then thiocyanate is added for crystallization; an acetate solution is added in a variable flow manner in a crystallization process; and a crystalline liquid is separated, subjected to elution and dried. The content of erythromycin A in erythromycin thiocyanate obtained by crystallization in the method is high; impurity erythromycin B and C are low in content; less erythromycin is destroyed in a separation and extraction process; and the yield of erythromycin A obtained by the crystallization is high.

Description

technical field [0001] The invention belongs to the technical field of biology and new medicine, and specifically relates to a method for extracting crystalline erythromycin thiocyanate from a fermentation liquid, in particular, adopting an ultrafiltration membrane to separate the fermentation liquid, and using a mixed solvent to extract the crystalline erythromycin thiocyanate Methods. Background technique [0002] Erythromycin is a class of macrolide antibiotics, mainly including erythromycin A, erythromycin B, erythromycin C, erythromycin D, erythromycin E, and erythromycin F. Among them, erythromycin A has the strongest antibacterial activity. Erythromycin is usually produced by microbial fermentation. The erythromycin in the fermentation broth mainly exists in the form of salt. At present, there are two main processes for extracting erythromycin in the fermentation broth, as follows: [0003] Process 1: microfiltration of fermentation broth; impurity removal by resin ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/08C07H1/06
Inventor 李学兵孙瑞君王良
Owner NINGXIA QIYUAN PHARMA
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