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A kind of method for preparing high-purity milbexime

A high-purity technology of mirbe oxime, applied in the field of animal pharmacy, can solve the problems of difficulty of mirbe oxime, many components and impurities, low product content, etc., and achieves the effect of rapid industrialized large-scale production, low equipment requirements and good versatility

Active Publication Date: 2017-12-12
CHONGQING DAXIN PHARMA +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, milbemycin is mainly obtained by semi-synthesis of milbemycin obtained by fermentation, but the unit of milbemycin fermentation broth is generally not high, the content of the product is low, the components have many impurities, and separation is difficult
This brings great difficulty to the preparation of high-purity milbexime

Method used

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  • A kind of method for preparing high-purity milbexime

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Experimental program
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Effect test

Embodiment 1

[0026] Plate-and-frame pressure filtration is performed on the fermentation broth containing milbemycin A3 and milbemycin A4 components, and the slag is extracted with toluene 8 times the weight of the slag, and the obtained toluene extract is detected by high-pressure liquid chromatography to calculate the content of milbemycin Beamycin component 100g. The toluene extract was concentrated until the content of the milbemycin component in the toluene was 15 g / L, and the toluene extract concentrate was filtered through a 0.45 μm pore size sterilizing plate.

[0027] The filtered toluene extract was loaded onto a silica gel column. The silica gel column is filled with 5kg of dry silica gel, and the silica gel particle size is 100-200 mesh. After the column is loaded, the silica gel column is analyzed with the desorbent of toluene:acetone=95:5 (V / V). The stripping liquids were combined, and the obtained stripping liquid contained 90 g of the milbemycin component. A small part of...

Embodiment 2

[0035] Plate and frame pressure filtration is carried out on the fermentation liquid containing milbemycin A3 and milbemycin A4 components, the bacteria residue is extracted with heptane 10 times the weight of the bacteria residue, and the obtained heptane extract is detected and calculated by high pressure liquid chromatography Contains milbemycin component 120g. The heptane extract was concentrated until the content of the milbemycin component in the heptane was 10 g / L, and the heptane extract concentrate was filtered through a sterilizing plate with a 0.2 μm pore size.

[0036] The filtered heptane extract was loaded onto a silica gel column. The silica gel column is filled with 12kg of dry silica gel, and the silica gel particle size is 300-400 mesh. After the column loading is completed, analyze the silica gel column with the desorbent of heptane: butanone = 80:20 (V / V). The stripping liquids were combined, and the obtained stripping liquid contained 110 g of the milbem...

Embodiment 3

[0044] Plate and frame pressure filtration is carried out on the fermentation liquid containing milbemycin A3 and milbemycin A4 components, and the bacterial residue is extracted with heptane 9 times the weight of the bacterial residue, and the obtained heptane extract is detected and calculated by high pressure liquid chromatography Contains milbemycin component 150g. The heptane extract was concentrated until the content of the milbemycin component in the heptane was 13 g / L, and the heptane extract concentrate was filtered through a sterilizing plate with a 0.2 μm pore size.

[0045] The filtered heptane extract was loaded onto a silica gel column. The silica gel column is filled with 15kg of dry silica gel, and the silica gel particle size is 100-200 mesh. After the column loading is completed, analyze the silica gel column with the desorbent of heptane: acetone = 90:10 (V / V). The stripping liquids were combined, and the obtained stripping liquid contained 128 g of the mi...

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Abstract

The invention discloses a method for preparing high-purity milbemycin. After extracting milbemycin A3 and milbemycin A4 from fermentation broth and preliminarily purifying them, they are oxidized with an oxidizing agent with low oxidation activity and subjected to silica gel chromatography. Increase the content of milbemycin A3 ketone and milbemycin A4 ketone from less than 25% to more than 75%, and naturally precipitate crystals during the concentration process, making milbemycin A3 ketone and milbemycin A4 ketone The content of milbemycin A3 oxime and milbemycin A4 oxime is adjusted to be 1:4 by resin chromatography, and the content of the product can be improved to More than 98%. The whole process is relatively simple, requires less equipment, has good versatility, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of animal pharmacy, and relates to a method for producing antibiotics for animals, in particular to a method for preparing high-purity milbexime. Background technique [0002] Milbemycin oxime is a new type of semi-synthetic macrolide anthelmintic drug, which is the oximated derivative of milbemycin A3 and A4, which is effective in controlling and preventing most common parasitic diseases. very good result. It is usually used to prevent heartworm disease, control dog and cat diseases caused by nematodes and hookworms, and whipworm disease in dogs. [0003] The chemical structural formulas of Milbe A3 oxime and Milbe A4 oxime are as follows: [0004] [0005] At present, milbemycin is mainly obtained by semi-synthesis of milbemycin obtained by fermentation, but the unit of milbemycin fermentation broth is generally not high, the content of the product is low, the components have many impurities, and separation is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/22
Inventor 何勇崴谢云张洪兰
Owner CHONGQING DAXIN PHARMA
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