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Demeclocycline extraction process

A technology of chlortetracycline and extraction process, applied in organic chemistry, separation/purification of carboxylic acid amides, etc., can solve the problems of product quality and yield impact, greatly increased environmental treatment cost, serious three waste discharge, etc. Stable guarantee of quality and yield, good economic and social benefits, and the effect of reducing the use of organic solvents

Inactive Publication Date: 2015-03-18
HENAN TOPFOND PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional method of fermenting and producing demeclotetracycline is to pretreat the demeclotetracycline fermentation liquid, filter after the plate and frame, extract the filtrate with butyl acetate and butanol, then use hydrochloric acid back extraction to concentrate, recrystallize, and bake. Dried to obtain demeclocycline hydrochloride, the traditional process uses a large amount of butyl acetate and butanol, and the two solvents have high water solubility, so the discharge of three wastes is serious, and the cost of environmental treatment is greatly increased; and due to the fermentation liquid Complexity and limitations of organic solvent extraction, resulting in difficult extraction, product quality and yield are affected differently

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 35 liters of fermentation broth containing 6.0g / L norchlortetracycline, adjust the temperature to 5-10°C, add 35g of 0.05wt% sodium sulfite, adjust the temperature to 10°C, use oxalic acid to adjust pH=1.5±0.2, stir for 20 minutes, Use the ceramic membrane filtration of Nanjing Jiuwu Company, the ceramic membrane flux is 30 liters / hour; the filtrate is 70 liters;

[0016] Pass the filtrate through 122 resin with a flow rate of 2BV / h. After completion, use drinking water with pH=6.8-7.0 to wash for 0.5 hours to obtain 72 liters of decolorizing liquid;

[0017] Pass the decolorizing liquid through the organic nanofiltration membrane module of GE Company of the United States with a molecular weight cut-off of 150 Daltons, the pressure is 1.5 mpa, and the temperature is maintained at 5-10 ℃; 4 liters of concentrated liquid is obtained;

[0018] Under the condition of stirring the concentrated solution, adjust the temperature to 5-8℃, use 0.1M ammonia water to adjust the pH=6.5...

Embodiment 2

[0021] Add 30 liters of fermentation broth containing 7.5g / L norchlortetracycline, add 150g of 0.5wt% sodium sulfite, adjust the temperature to 5-10°C, use hydrochloric acid to adjust pH=2.5±0.2, stir for 20 minutes, use Xiamen Sanda Company Ceramic membrane filtration, ceramic membrane flux 24.5 liters / hour; 65 liters of filtrate;

[0022] Decolorize the filtrate through LX-200 resin at a flow rate of 3BV / h. After completion, use drinking water with pH=6.8-7.0 for top washing for 0.5 hours to obtain 70 liters of decolorizing liquid;

[0023] Pass the decolorizing liquid through the organic nanofiltration membrane module of GE Company of the United States with a molecular weight cut-off of 150 Daltons, the pressure is 1.5 mpa, and the temperature is maintained at 5-10 ℃; 3.8 liters of concentrated liquid are obtained;

[0024] Under the condition of stirring the concentrated solution, adjust the temperature to 5-8℃, use 2M NaOH aqueous solution to adjust the pH=8.2±0.2 to obtain th...

Embodiment 3

[0027] Add 30 liters of fermentation broth containing 5.8g / L norchlortetracycline, adjust the temperature to 5-10℃, add 30g of 0.1wt% sodium sulfite, adjust pH=3.8±0.2 with oxalic acid, stir for 20 minutes, use Nanjing Jiuwu Company Ceramic membrane filtration, ceramic membrane flux 28.5 liters / hour; 70 liters of filtrate;

[0028] Pass the filtrate through Rohm and Haas decolorizing resin at a flow rate of 4BV / h. After completion, use drinking water with pH=6.8-7.0 to wash for 0.5h to obtain 75 liters of decolorizing liquid;

[0029] Pass the decolorizing liquid through the organic nanofiltration membrane module of American GE company with a molecular weight cut-off of 100 Dalton, the pressure is 1.8mpa, and the temperature is maintained at 5-10℃; 4.5 liters of concentrated liquid is obtained;

[0030] Under the condition of stirring the concentrated solution, adjust the temperature to 5-8℃, use 1M ammonia water to adjust the pH=4.8±0.2 to obtain the precipitation suspension, cont...

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PUM

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Abstract

The invention provides a demeclocycline extraction process which comprises the following technical steps: adding an antioxidant into demeclocycline fermentation liquor, adjusting the pH to 1.0-4.0 by an acid, micro-filtering to separate mycelia and other solid impurities, and decolorizing the filtrate; concentrating the decolorized filtrate by using a nanofiltration organic film to obtain a demeclocycline concentrated solution; adjusting the pH of the concentrated solution to 4.5-8.5 by an alkali, carrying out crystallization and sedimentation, and carrying out solid-liquid separation on precipitate to obtain a demeclocycline crude product; and refining the demeclocycline crude product by using a double salt method to obtain a demeclocycline hydrochloride finished product. Compared with the original solvent extraction process, the process provided by the invention avoids use of organic solvents or greatly reduces use of organic solvents, so that discharge of three wastes is less and the environmental pollution is reduced. The process is stable in product yield and quality and suitable for industrial production and has a very high practical value. The obtained product meets EP and USP standards.

Description

Technical field [0001] The invention relates to the preparation of medicines, in particular to a new extraction process of norchlortetracycline. Background technique [0002] Norchlortetracycline, also known as demecycline, desmethylchlorotetracycline, etc., is a tetracycline antibiotic produced by the fermentation of Streptomyces aureus. Its antibacterial spectrum is similar to that of chlortetracycline, and its antibacterial effect is stronger than tetracycline. More stable than chlortetracycline. With the successive listings of the derivatives minocycline and tigecycline and the continuous development of other derivatives, the market prospect of norchlortetracycline is becoming more and more broad. [0003] The traditional fermentative production and extraction method of norchlortetracycline is to pretreat the fermentation broth of norchlortetracycline, filter after plate and frame, and extract the filtrate with butyl acetate and butanol, and then use hydrochloric acid to back ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C237/26C07C231/24
Inventor 刘俭国毛全贵焦龙孟新梅祝立新王九唐慧慧牛景丽孟利沙王媛王雪洁谢书琴万丹刘丽杰王丹
Owner HENAN TOPFOND PHARMA