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Method for separating and purifying milbemycins fermentation liquor

A milbemycin, separation and purification technology, applied in the direction of organic chemistry, can solve the problems of human body and environment, low yield, low purity, etc., and achieve the effect of promoting flocculation, reducing burden, and improving flocculation efficiency

Active Publication Date: 2021-02-23
内蒙古拜克生物有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this invention, the purity and yield of milbemycin are high, but in this method, acetone and other toxic substances need to be used as the eluent, which will have adverse effects on the human body and the environment.
[0005] Aiming at the defects such as low purity, low yield and harm to human body and environment in the separation and purification method of the existing milbemycin fermentation liquid, it is urgent to find a separation and purification method to obtain high-purity milbemycin At the same time, it can also avoid the reduction of the yield and the harm to the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A method for separating and purifying a milbemycin fermentation broth, comprising the following steps:

[0031] (1) Fermentation broth pretreatment: after heating and insulating the milbemycin fermentation broth, through flocculation and filtration, to obtain mycelial slag;

[0032] The flocculant used in the flocculation process is diatomite-polymeric ferric sulfate-modified activated carbon composite flocculant;

[0033] The preparation method of the diatomite-polymeric ferric sulfate-modified activated carbon composite flocculant comprises the following steps: adding ferric citrate into water, heating to 60°C and stirring and dissolving to a viscous state to obtain a mass fraction of 8% Add ferric citrate solution, then add activated carbon for impregnation for 24 hours. The amount of ferric citrate solution used is based on the amount that can completely submerge the activated carbon. Dry and activate and pyrolyze at 600°C for 1 hour to obtain modified activated car...

Embodiment 2

[0039] A method for separating and purifying a milbemycin fermentation broth, comprising the following steps:

[0040] (1) Fermentation broth pretreatment: after heating and insulating the milbemycin fermentation broth, through flocculation and filtration, to obtain mycelial slag;

[0041] The flocculant used in the flocculation process is diatomite-polymeric ferric sulfate-modified activated carbon composite flocculant;

[0042]The preparation method of the diatomite-polymeric ferric sulfate-modified activated carbon composite flocculant comprises the following steps: adding ferric citrate into water, heating to 80° C. and stirring and dissolving to a viscous state to obtain a mass fraction of 10% Add ferric citrate solution, then add activated carbon for impregnation for 24 hours, the usage of ferric citrate solution shall be based on the amount that can completely immerse the activated carbon, dry and activate and pyrolyze at 700°C for 0.5h to obtain modified activated carb...

Embodiment 3

[0048] A method for separating and purifying a milbemycin fermentation broth, comprising the following steps:

[0049] (1) Fermentation broth pretreatment: after heating and insulating the milbemycin fermentation broth, through flocculation and filtration, to obtain mycelial slag;

[0050] The flocculant used in the flocculation process is diatomite-polymeric ferric sulfate-modified activated carbon composite flocculant;

[0051] The preparation method of the diatomite-polymeric ferric sulfate-modified activated carbon composite flocculant comprises the following steps: adding ferric citrate into water, heating to 70° C. and stirring and dissolving to a viscous state to obtain a mass fraction of 9% Add ferric citrate solution, then add activated carbon for impregnation for 24 hours. The amount of ferric citrate solution used is based on the ability to completely submerge the activated carbon. Dry and activate and pyrolyze at 650°C for 0.8 hours to obtain modified activated car...

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Abstract

The invention provides a method for separating and purifying milbemycins fermentation liquor, and relates to the field of biological fermentation pharmacy, and the method comprises the following steps: (1) pretreatment on the fermentation liquor: heating and insulating the milbemycins fermentation liquor, flocculating and filtering to obtain mycelium residues, wherein a flocculating agent used inthe flocculation process is a diatomite-polyferric sulfate-modified activated carbon composite flocculating agent, (2) primary purification: drying the mycelium residues, adding absolute ethyl alcohol, stirring and filtering to obtain filtrate, concentrating under reduced pressure to obtain extract, and adding an ethanol solution to obtain a crude extract, (3) high purification: adsorbing the crude extract by using macroporous resin, removing impurities, and eluting by using an ethanol solution to obtain a refined extract, and (4) crystallizing and drying: crystallizing, centrifuging and drying the refined extract to obtain milbemycins. The milbemycins fermentation liquor is separated and purified through the process, so that the product yield can be increased, and the product quality canbe guaranteed.

Description

technical field [0001] The invention relates to the field of biofermentation pharmaceuticals, in particular to a method for separating and purifying milbemycin fermentation broth. Background technique [0002] Milbemycin is a micro-antibiotic isolated from fermentation broth with a mixture of hexadecyllides. It has excellent biological activities such as insecticidal, acaricidal, anthelmintic and anti-tumor. Milbemycin is in It is a biopesticide with relatively broad spectrum, high efficiency and no cross-resistance to insects. Therefore, the preparation of high-purity, high-yield milbemycin is of great significance. [0003] At present, most of the separation and purification methods related to milbemycin use methanol and other solvents for leaching, such as literature: Chen Xiaolong, Zheng Yuguo, Shen Yinchu. Research progress of biological pesticide milbemycin [J]. Pesticides, 2003, 42(4 ): 5-5. But methanol and other solvents have certain toxicity, consume a large amou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/22
CPCC07D493/22
Inventor 陈峰钟迎东叶朋马贵军宫颖章
Owner 内蒙古拜克生物有限公司
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