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Purification method for Nemadectin

A purification method and organic solvent technology, applied in the field of animal pharmacy, can solve the problems of high recovery cost of rectification, expensive chromatography column, high one-time investment, reduce energy consumption and production cost, facilitate the expansion of production scale and equipment. low investment

Active Publication Date: 2014-05-07
NEW FOUNDER HLDG DEV LLC +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method has the disadvantages of high resin price and supporting chromatographic column, high one-time investment, huge amount of organic solvent used in chromatography, and high rectification recovery cost.
[0006] In addition, in the Chinese patent application 201010237843.5, the fermented liquid containing nimoctine is processed by spray drying because it is difficult to press filter. Although this method can obtain dry and fluffy bacteria residues for easy extraction, the power cost of this method is high. Higher cost of mass production

Method used

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  • Purification method for Nemadectin

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1. After the streptomycin fermentation broth is put into the tank, an anionic polyacrylamide flocculant solution is added to it, and added according to the ratio of 0.01 to 0.02 g / L fermentation broth, stirred evenly, press-filtered, topped with water, and dried to obtain 4285g of fungus residue, wherein the content of nemoctine is 60g, and the content is 57%.

[0034] 2. Use 25L of 60% aqueous ethanol solution to carry out stirring extraction on the filter press bacterial residue, the extraction temperature is 40-50° C., extract for 4 hours and then separate. A total of three extractions were performed. The first two mergers have a total of 54g of nemoctine, with a content of 68%; the third time is applied to the next Yicui.

[0035] 3. After combining the two extracts, add water, reduce the concentration of ethanol to 40-50%, then add 13L of dichloromethane for extraction, stir and extract for 2 hours, then stand and separate. Extraction was done twice, the second h...

Embodiment 2

[0039] 1. After putting the streptomycin fermentation broth into the tank, add polyaluminum sulfate solution in a ratio of 0.1 to 0.5g / L fermentation broth, stir evenly, press filter, top water, and dry to obtain 3856g of fungus residue , wherein the content of nemoctine is 46g, and the content is 60%.

[0040] 2. Use 20 L of 40% acetone aqueous solution to carry out stirring extraction on the filter press bacterial residue, the extraction temperature is 40-50° C., extract for 4 hours and then separate. A total of three extractions were performed. The first two mergers have a total of 42g of nemoctine, with a content of 71%; the third time is applied to the next Yicui.

[0041] 3. Combine the two extracts, add water, reduce the concentration of acetone to 30%, then add 20 L of toluene for extraction, stir and extract for 2 hours, and then stand for separation. Extracted twice, the second toluene extraction was used for the next extraction.

[0042] 4. Concentrate the toluen...

Embodiment 3

[0045] 1. After the streptomycin fermentation broth is put into the tank, add calcium chloride-sodium dihydrogen phosphate combined solution, add according to the ratio of 10g calcium chloride+6g disodium hydrogen phosphate / L fermentation broth, stir evenly and press Filter, top water, blow dry, obtain bacterium residue 4025g, wherein the content of nimoctine is 52g, and content is 58%.

[0046] 2. Use 20 L of 80% methanol aqueous solution to carry out stirring extraction on the filter press bacterial residue, the extraction temperature is 40-50° C., extract for 4 hours and then separate. A total of three extractions were performed. The first two mergers have a total of 50 g of nemoctine, with a content of 66%; the third time is applied to the next Yicui.

[0047] 3. After combining the two extracts, add water, reduce the concentration of methanol to 40-50%, and then add 10 L of ethyl acetate for extraction, stir and extract for 2 hours, then stand and separate. Extract twic...

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Abstract

The invention provides a purification method for Nemadectin. The method comprises the following steps: performing filter pressing on flocculated Nemadectin-containing fermentation liquid to obtain filter press bacteria dregs; extracting the filter press bacteria dregs by using the aqueous solution of a first solvent to obtain a Nemadectin-containing extract; stripping the extract by using a second solvent to obtain a Nemadectin-containing stripping liquid, wherein the polarity of the second organic solvent is weaker than that of the first organic solvent; concentrating the stripping extract and crystallizing to obtain the purified Nemadectin. According to the purification method for the Nemadectin, all of the adopted separation and purification means are conventional separation means in bio-pharmacy; equipment has high universality and low cost; moreover, the production operation is simple and convenient, the production operating cost is low, and the enlargement of production scale is facilitated.

Description

technical field [0001] The invention belongs to the field of animal pharmacy, and relates to a method for purifying antibiotics for animals, in particular to a method for purifying nemoctine. Background technique [0002] Nemadectin is a sixteen-membered macrolide antibiotic that can be produced by Streptomycescyaneogriseus sp. Noncyanogenus through fermentation. As a member of Milbemycin, Nimoctine is mainly used to synthesize the more active anthelmintic drug Moxidectin. The chemical structure of Nimoctin is as follows: [0003] [0004] Nimoctine [0005] Chinese patent application 200810126358.3 describes a method for purifying nimoctine through a macroporous resin. In the Chinese patent application 201010237843.5, the HPLC purity of nimoctine reaches more than 90% by chromatography with HP20SS macroporous resin produced by Mitsubishi Chemical. However, this method has the disadvantages of high resin price and supporting chromatographic column, high one-time inves...

Claims

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Application Information

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IPC IPC(8): C07H19/01C07H1/06
Inventor 何勇崴张洪兰
Owner NEW FOUNDER HLDG DEV LLC
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