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Preparation method of spiramycin adipate

A technology of spiramycin adipate and spiramycin, which is applied in the field of medicine, can solve problems such as unstable product quality, high waste water pollutants, and large energy consumption, so as to reduce environmental pollution and personal hazards, and reduce waste liquid discharge , high potency effect

Pending Publication Date: 2021-09-10
TOPFOND PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, in the actual preparation process, the production of spiramycin first will result in higher levels of wastewater pollutants; the use of methanol for treatment will easily cause environmental pollution and human hazards; the subsequent distillation and drying process requires high temperature, long time, and large energy consumption; finally, The quality of the obtained product is unstable, and the appearance is slightly yellow

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] (1) Get spiramycin fermentation filtrate, adjust pH9.28 with 10% sodium hydroxide solution, centrifuge for 5 minutes, control speed 5000r / min; get supernatant 10L, titer 14681μ / ml, supernatant billion 0.146 billion . Add 1.2L of butyl acetate to the supernatant for extraction, the extraction temperature is 30°C, stir for 10 minutes, let stand for stratification for 40 minutes, and collect the extract phase; add 200ml of saturated brine for stirring for 10 minutes, and let stand for stratification for 40 minutes to obtain spiramycin Extract 1.15L, titer 116824μ / ml (0.134 billion);

[0044] (2) In the obtained spiramycin extract in step (1), add 1.3% adipic acid solution to adjust the pH5.50, stir for 40min, then let stand for stratification, and the lower layer solution is adipate spiramycin solution 0.27 L, titer 471481 μ / ml (0.127 billion);

[0045] (3) Add 0.27 g of activated carbon to the adipate spiramycin obtained in step 2, stir for 40 minutes at a temperature o...

Embodiment 2

[0048] (1) Get spiramycin fermentation filtrate, adjust pH9.32 with 10% sodium hydroxide solution, centrifuge for 5 minutes, control speed 5000r / min; get supernatant 10L, supernatant titer 12358μ / ml, supernatant 0.123 billion. Add 1.2 L of butyl acetate to the supernatant for extraction, the extraction temperature is 30°C, stir for 10 minutes, let stand for 40 minutes to separate the layers, and collect the extract phase; add 240 ml of saturated brine to stir for 10 minutes, then stand for 40 minutes to separate the layers to obtain spiramycin Extract 1.08L, titer 100000μ / ml (0.108 billion);

[0049] (2) In the obtained spiramycin extract in step (1), add 1.3% adipic acid solution to adjust the pH to 5.32, stir for 40 min, then let stand for stratification, and the lower layer solution is adipate spiramycin solution 0.22 L, titer 475000μ / ml (0.104 billion);

[0050] (3) Add 0.25 g of activated carbon to the adipate spiramycin obtained in step 2, stir for 40 minutes at a temp...

Embodiment 3

[0053] (1) Get the spiramycin fermentation filtrate, adjust the pH to 9.16 with 10% sodium hydroxide solution, centrifuge for 5 minutes, and control the rotating speed at 5000r / min; get 10L of supernatant, titer 11246μ / ml, supernatant 0.112 billion. Add 1.0L of butyl acetate to the supernatant for extraction, the extraction temperature is 30°C, stir for 10 minutes, let stand for stratification for 40 minutes, and collect the extract phase; add 200ml of saturated brine for stirring for 10 minutes, then stand for stratification for 40 minutes to obtain spiramycin Extract 0.95L, titer 97864μ / ml (0.093 billion);

[0054] (2) In the obtained spiramycin extract in step (1), add 1.3% adipic acid solution to adjust the pH to 5.03, stir for 40 min, then let stand for stratification, and the lower layer solution is adipate spiramycin solution 0.24 L, titer 368125μ / ml (0.088 billion);

[0055] (3) Add 0.25 g of activated carbon to the adipate spiramycin obtained in step 2, stir for 40 m...

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Abstract

The invention provides a preparation method of spiramycin adipate, and relates to the technical field of medicines. The preparation method specifically comprises the following steps that spiramycin fermentation filtrate serves as a raw material, the pH of the filtrate is adjusted, centrifugation is conducted, supernate is taken and added into n-butyl acetate, uniform stirring, mixed extraction, standing layering and organic phase collection are conducted, and spiramycin extracting solution is obtained; an adipic acid solution is into the spiramycin extracting solution, the pH value is adjusted, back extraction is conducted onthe solution, stirring, standing, and layering are conducted, and a lower phase is taken so as to obtain a back extraction solution; activated carbon is added into the back extraction liquid, and fully stirring and decoloring are conducted to obtain a decolored liquid; and drying and crystallizing the decolored solution are conducted to obtain a finished product of the spiramycin adipate. According to the spiramycin adipate prepared by the method, the finished product of the spiramycin adipate is directly prepared from the spiramycin fermentation filtrate. According to the invention, crystallization and drying links are reduced in the spiramycin preparation process, the product yield is improved, and the method has the characteristics of good product character, safe operation, energy consumption saving and waste liquid discharge reduction.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a preparation method of spiramycin adipate. The invention also provides a method for preparing spiramycin adipate which is suitable for industrial production. Background technique [0002] Spiramycin, English name Spiramycin, is a multi-component macrolide antibiotic produced by S. ambofacienss. It is a white or slightly yellow powder with a slight odor; slightly hygroscopic; easily soluble in ethanol , propanol, acetone and methanol, insoluble in water. Spiramycin belongs to the 16-membered macrolide antibiotics. In actual production, the finished product of spiramycin is mainly extracted after microbial fermentation. [0003] In the existing spiramycin extraction technology, the commonly used method is: filter the spiramycin fermentation liquid after pretreatment to obtain the spiramycin filtrate, and then add a neutral organic solvent in the spiramycin filtrate, ...

Claims

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Application Information

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IPC IPC(8): C07H1/06C07H17/08C07C51/47C07C51/43C07C55/14
CPCC07H1/06C07H17/08C07C51/47C07C51/43C07C55/14
Inventor 刘守强陈晓东周淑梅徐文斌李海剑刘建超谢芝丽王辉张宏周陈中刚管勇王雪洁张钦林刘果
Owner TOPFOND PHARMA CO LTD
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