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A method of preparing high-purity milbemycin oxime

A Mirbeoxime, high-purity technology, applied in the field of animal pharmacy, can solve the problems of difficulty of mirbeoxime, many components and impurities, difficult separation, etc., and achieves the effects of rapid industrialized large-scale production, low equipment requirements and simple process.

Active Publication Date: 2016-03-30
CHONGQING DAXIN PHARMA +2
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  • Summary
  • Abstract
  • Description
  • Claims
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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 method of preparing high-purity milbemycin oxime

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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

A method of preparing high-purity milbemycin oxime is disclosed. The method includes extracting milbemycin A3 and milbemycin A4 from a fermentation liquor, performing preliminary purification, oxidizing with an oxidant low in oxidizing activity, performing silica gel chromatography to increase the content of milbemycin A3 ketone and milbemycin A4 ketone to a value higher than 75% from a value lower than 25%, naturally crystallizing during concentration to increase the content of the milbemycin A3 ketone and the milbemycin A4 ketone to a value higher than 95%, performing oximation, and performing resin chromatography to adjust the ratio of the content of milbemycin A3 oxime to the content of milbemycin A4 oxime to be 1:4 and to increase the product purity to be higher than 98%. The method is simple in process, low in equipment requirement, good in universality and suitable for large-scale 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] Milbemycinoxime (milbemycinoxime) is a new type of semi-synthetic macrolide anthelmintic drug, which is the oximated derivative of milbemycin A3 and A4. Good results. 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 difficult. This brings great difficulty to the preparation of high-...

Claims

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Application Information

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IPC IPC(8): C07D493/22
Inventor 何勇崴谢云张洪兰
Owner CHONGQING DAXIN PHARMA
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