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A kind of separation and purification method of milbemycin fermented liquid

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

Active Publication Date: 2021-09-28
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 a milbemycin fermented liquid, which relates to the field of biological fermentation and pharmacy. , filter to obtain mycelium slag; the flocculant used in the flocculation process is diatomite-polyferric sulfate-modified activated carbon composite flocculant; (2) preliminary purification: after the mycelium slag is dried, add dehydrated alcohol, Stir and filter to obtain the filtrate, concentrate under reduced pressure to obtain the extract, add ethanol solution to obtain the crude extract; (3) Highly purified: use the macroporous resin to load the sample crude extract for adsorption, and elute with ethanol solution after removing impurities to obtain Extract; (4) crystallization and drying: crystallize, centrifuge and dry the extract to obtain milbemycin. Separating and purifying the milbemycin fermentation broth through the above process can improve the yield of the product while ensuring the quality of the product.

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 Patents(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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