Preparation method of abamectin

A technology of abamectin and crude product, applied in the field of preparation of high-purity abamectin, can solve problems such as not suitable for large-scale production and application, no obvious removal effect of impurities, unsatisfactory removal effect of impurities, etc., and achieve low production cost , less investment in equipment, and improved elution efficiency

Active Publication Date: 2016-12-07
NORTH CHINA PHARMA GROUP AINO
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This type of process is easy to operate and can be used for large-scale production, but the effect of removing impurities is not ideal. It needs repeated crystallization many times to obtain high-purity abamectin products, and has no obvious removal effect on some impurities.
Another type of preparation process mainly adopts the method of column separation to obtain high-purity avermectin fine powder. This type of process has the advantages of good impurity removal effect, but the production cost is high and the investment in equipment is high, so it is not suitable for large-scale production application

Method used

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  • Preparation method of abamectin
  • Preparation method of abamectin
  • Preparation method of abamectin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Preparation of crude abamectin.

[0034] The Streptomyces avermitilis strain was inoculated on the slant medium, and cultured for 10 days at 28° C. and an ambient relative humidity of 55%. Dig out the lawn from the inclined surface, insert it into the sterilized seed medium, and cultivate it for 48 hours at 28°C, the relative humidity of the environment is 55%, the cultivation speed is 200rpm, and the rotation radius is 50mm to obtain the seed solution. Inoculate the seed liquid with an inoculation amount of 5% by volume in a 50L fermenter equipped with fermentation medium. The tank temperature is 28°C, the relative humidity of the environment is 55%, the tank pressure is 0.05±0.01Mpa, the ventilation rate is 20L / min, and 200rpm is stirred. Fermentation 240h ​​obtains the abamectin fermented liquid.

[0035] The preparation method of the slant medium is: glucose 15g, beef extract 3g, asparagine 0.5g, KH 2 PO 4 0.5g, agar 19g, add tap water to dissolve to 1000ml, pH v...

Embodiment 2

[0040] Get 10g Abamectin crude product, adopt 30ml of organic solvent dissolving according to every gram Abamectin crude product, select toluene as organic solvent, add 300ml toluene in Abamectin crude product, dissolve at 50 ℃, be mixed with crude product solution.

[0041]Take sodium sulfate, absolute ethanol and water and prepare the eluent, specifically: at a dissolution temperature of 25°C, add water to 90ml of absolute ethanol to 300ml to prepare an aqueous ethanol solution, then add 3g of sodium sulfate to the aqueous ethanol solution, Dissolve and prepare as eluent.

[0042] Elution was carried out in a countercurrent extraction equipment, the elution ratio of the crude product solution to the eluent was 1:1, the elution temperature was set at 25°C, the flow rate of the crude product solution was 7ml / min, and the flow rate of the eluent was 7ml / min , after the elution is complete, the eluate is obtained.

[0043] The eluate was concentrated and dried, and the dried pr...

Embodiment 3

[0045] Get 15g Abamectin crude product, adopt 30ml organic solvent dissolving according to every gram Abamectin crude product, select sec-butyl acetate as organic solvent, add 450ml sec-butyl acetate in Abamectin crude product, 50 ℃ dissolve, Prepared as a crude solution.

[0046] Take sodium carbonate, anhydrous methanol and water to prepare the eluent, specifically: at a dissolution temperature of 30°C, add water to 135ml of anhydrous methanol to 450ml to prepare methanol aqueous solution, and then add 4.5g of sodium carbonate to the methanol aqueous solution , dissolved clear, prepared as eluent.

[0047] Elution was carried out in a countercurrent extraction equipment, the elution ratio of the crude product solution to the eluent was 1:1, the elution temperature was set at 25°C, the flow rate of the crude product solution was 14ml / min, and the flow rate of the eluent was 14ml / min , after the elution is complete, the eluate is obtained.

[0048] The eluate was concentrate...

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Abstract

The invention discloses a preparation method of abamectin. The preparation method comprises the following steps: (1) dissolving an abamectin crude product by adopting an organic solvent to obtain a crude product solution; (2) taking inorganic salt, a polar solvent and water and preparing an eluent with a certain concentration and eluting the crude product solution by utilizing the eluent in a counter-current extraction tower to obtain an eluting solution; (3) concentrating and drying the eluting solution, and recrystallizing a dried product to obtain a pure abamectin product. By introducing a counter-current extraction technology into an abamectin purification process, the eluting efficiency is greatly improved; large-polarity impurities can be effectively removed and continuous operation of a purification process is realized; the preparation method of the abamectin has the advantages of small equipment investment, simplicity in operation, relatively high yield, low production cost, capability of being industrially produced in a large scale and the like.

Description

technical field [0001] The invention belongs to the technical field of industrial microbes, and in particular relates to a method for preparing high-purity abamectin from a crude avermectin produced from a fermentation culture. Background technique [0002] The existing preparation process of abamectin fine powder mainly uses an organic solvent to dissolve the abamectin, and then conducts cooling and crystallization to obtain abamectin fine powder. This type of process is easy to operate and can be used for large-scale production, but the effect of removing impurities is not ideal. It needs repeated crystallization for many times to obtain high-purity abamectin products, and has no obvious removal effect on some impurities. Another type of preparation process mainly adopts the method of column separation to obtain high-purity abamectin fine powder. This type of process has the advantage of good impurity removal effect, but the production cost is high and the investment in eq...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08C07H1/06C12P19/62
CPCC07H1/06C07H17/08C12P19/623
Inventor 孙耀华刘书琴王文华张宾张丽强龙燕耿焕敏李学红王兴轩张芳
Owner NORTH CHINA PHARMA GROUP AINO
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