Method for separating and purifying spiramycin by utilizing alkylphenol polyoxyethylene polyoxypropylene ether NPE-108

A technology of alkylphenol polyoxyethylene polyoxypropylene ether and spiramycin, which is applied in the fields of organic chemistry, chemical instruments and methods, preparation of sugar derivatives, etc., can solve the problem of immature synthesis process, long phase formation time, polymer High cost and other problems, to achieve the effect of easy industrial application, reduce separation cost, and reduce purification cost

Active Publication Date: 2021-02-19
EAST CHINA UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this separation and purification method is currently only in the laboratory stage, because the two-phase aqueous system constructed by using two responsive polymer...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1 NPE-108 / Water Temperature Induced Reproducible Two-phase System Normal Extraction Experiment of Spiramycin

[0017] Filter and centrifuge the spiramycin fermentation broth for later use, add 20mL spiramycin fermentation broth to a 50mL graduated centrifuge tube, then add 4mL NPE-108 and mix well, adjust the pH of the solution to 9.0, and place it in a 55°C water bath Carry out the first normal extraction in the medium, after the distribution equilibrium is reached, separate the upper and lower phases, take 50uL of the upper and lower phases with a pipette gun, dilute to 1.0mL with ultrapure water, and measure the concentration of the upper and lower phases according to the known spiramycin liquid phase detection method. Concentration of spiramycin. Add 0.2 times the volume of NPE-108 to the upper phase obtained from the first normal extraction, adjust the pH to 9.0 after mixing, and place it in a 55°C water bath until the distribution equilibrium is reached. S...

Embodiment 2

[0018] Example 2 The experiment of NPE-108 / water temperature induced regenerable two-phase system back-extracting spiramycin

[0019] Mix the lower phase obtained from the two normal extractions in Example 1, add 0.25 times the volume of pure water, adjust the pH to 5.8 after shaking evenly, and place it in a 55°C water bath for back extraction. After reaching the distribution equilibrium, separate For the upper and lower phases, use a pipette gun to take 50uL each of the upper and lower phases, dilute to 1.0mL with ultrapure water, and measure the concentration of spiramycin in the upper and lower phases according to the known spiramycin liquid phase detection method. It is known that under this condition, the stripping partition coefficient of spiramycin reaches 35 in the NPE-108 / water temperature-induced reproducible two-phase aqueous system.

Embodiment 3

[0020] Example 3 The recovery experiment of thermoresponsive polymer NPE-108

[0021] The lower phase obtained by stripping in Example 2 was placed in a water bath at 60° C., and the upper aqueous solution was removed after standing for 30 minutes. The recovery rate of NPE-108 obtained was 98.8%.

[0022] In summary, the EOPO of the present invention 108 / Water temperature-induced regenerable two-phase aqueous system has the advantages of high water content, high recovery, short phase formation time, and simple operation. The separation and purification of the spiramycin in the fermented liquid by the invention has a good separation effect and is suitable for industrial application.

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Abstract

The invention relates to a method for separating and purifying spiramycin. Alkylphenol polyoxyethylene polyoxypropylene ether NPE-108 can be used for forming a two-aqueous-phase system to separate thespiramycin. The method is characterized in that during first forward extraction, NPE-108 and spiramycin fermentation liquor are mixed according to the volume ratio of 1: 5, the pH value is adjusted to be 9.0, the two-aqueous-phase system is formed through induction at the temperature of 55 DEG C, and after distribution equilibrium is achieved, the spiramycin in the fermentation liquor is distributed to an NPE-108 phase (a lower phase), an upper phase is separated, and the upper phase is used for second forward extraction; lower phases of the two times of forward extraction are mixed, pure water with 0.25 times of volume is added, the pH value is adjusted to be 5.8, distribution is condcuted at 55 DEG C, and the spiramycin enriched in the NPE-108 phase is reversely extracted into a water phase; the spiramycin can be separated from the fermentation liquor through two-stage forward extraction and one-stage reverse extraction; and the NPE-108 can be recovered through temperature adjustment, and the recovery rate reaches 98.8%. The method has the advantages of mild operation conditions, efficient recovery, safety and environmental protection and the like.

Description

technical field [0001] The present invention relates to the technical field of two-phase extraction, more specifically, relates to the technical field of temperature-induced regenerable two-phase extraction, in particular to the process design and process for separating and purifying spiramycin in fermentation broth by utilizing temperature-induced and regenerable two-phase system Process Optimization. Background technique [0002] Block polyether NPE-108 is a heat-sensitive polymer, which is obtained by modifying alkylphenol with block copolymer composed of monomers ethylene oxide (EO) and propylene oxide (PO). The molecular weight of the polymer is 0.79kDa, and the cloud point is 39°C. The cloud point of the polymer can be changed by adjusting the ratio of EO / PO in the polyether. When the NPE-108 aqueous solution is heated, the cloud point of the polymer is exceeded, and the solution becomes turbid. When the temperature continues to rise to 15°C above the cloud point, the...

Claims

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Application Information

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IPC IPC(8): C07H1/06C07H17/08
CPCC07H1/06C07H17/08
Inventor 曹学君万俊芬张燕王振平王艳杨婷魏艳丽张宏周贺栋
Owner EAST CHINA UNIV OF SCI & TECH
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