Production method of milbemycin

A technology of milbemycin and production method, applied in the direction of organic chemistry and the like, can solve the problems of large amount of solvent recovery, large amount of solvent used, poor stability, etc., and achieve the effects of high purity, high equipment cost and good stability

Active Publication Date: 2017-07-14
LIVZON GROUP FUZHOU FUXING PHARMACEUTICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The resin separation process of this production method generally takes 3 days, and the amount of solvent used is relatively large. It takes about 15 m to separate 10 kg of milbemycin in production. 3 T...

Method used

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  • Production method of milbemycin
  • Production method of milbemycin

Examples

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Effect test

Embodiment 1

[0061] A production method of milbemycin, comprising the following steps:

[0062] The present invention also provides a kind of production method of Milbemycin, comprising the following steps:

[0063] Step a: filtering the milbemycin fermentation liquid to obtain the bacterial residue;

[0064] Step b: adding acetone or ethanol to the fungus residue in step a for stirring and extraction, the liquid-to-solid ratio of the acetone or ethanol to the fungus residue is 6-10L: 3kg, the stirring time is 5-7h, and then filtered to obtain Milbemycin extract;

[0065] Step c: Concentrating the milbemycin extract in step b until the volume content of acetone or ethanol is 20-30%, to obtain milbemycin extract;

[0066] Step d: using the first solvent to dissolve the milbemycin extract obtained in step c to obtain the first milbemycin solution, wherein the ratio of the added amount of the first solvent to the bacterium residue in step b is 9 ~11L: 150kg;

[0067] Step e: Add the secon...

Embodiment 2

[0074] A kind of production method of milbemycin (production with 750kg bacterium residue as raw material, containing about 20kg of milbemycin), comprises the following steps:

[0075] Step a: filtering the milbemycin fermentation liquid to obtain the bacterial residue;

[0076] Step b: take 750kg of bacteria residue, put it into the extraction tank, add 2000L acetone, stir for 6h, and then filter to obtain the milbemycin extract;

[0077] Step c: Concentrating the milbemycin extract in step b until the volume content of acetone is 20-30%, to obtain milbemycin extract;

[0078] Step d: add 50L of acetone to the milbemycin extract obtained in step c to dissolve, and obtain the first milbemycin solution;

[0079] Step e: Slowly add 250L n-heptane to the first milbemycin solution in step d, control the flow rate of n-heptane addition to be 5.3-8.7L / min (completely added within 30-45min), and control the temperature at 20 ~30°C, stirred for 5 hours to crystallize, and filtered t...

Embodiment 3

[0084] A kind of production method of milbemycin (production with 750kg bacterium slag as raw material), operation steps are the same as embodiment 2, difference is that the acetone addition in step b is changed into 1500L, and stirring time is changed into 5h; The amount of acetone added in d and step f is changed to 45L; the amount of n-heptane added in step e and step g is changed to 240L, and the stirring and crystallization time is changed to 4.5h. Demilbemycin recrystallized powder 16.5kg.

[0085] The purity of the obtained milbemycin recrystallized powder determined by HPLC was 97.3%, and the yield was about 82.5%. Yield calculation method is the same as embodiment 1.

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Abstract

The invention provides a production method of milbemycin. The production method comprises the following steps: (S1) dissolving a milbemycin extract by virtue of a first solvent, so as to obtain a first milbemycin dissolving solution; (S2) adding a second solvent into the first milbemycin dissolving solution obtained in the step (S1), stirring to crystallize, so as to obtain coarse crystallization powder; (S3) dissolving the coarse crystallization powder obtained in the step (S2) with the first solvent, so as to obtain a second milbemycin dissolving solution; and (S4) adding the second solvent into the second milbemycin dissolving solution obtained in the step (S3), stirring to recrystallize, so as to obtain milbemycin recrystallization powder, wherein the first solvent is any one of ethanol, acetone, ethyl acetate or isopropyl-ketone, and the second solvent is any one of n-hexane, n-heptane, n-octane, n-nonane, n-decane, n-undecane or n-dodecane. The production method provided by the invention has the advantages that the process is simple, the production cycle is short, the recycling amounts of the solvents are low, and the prepared milbemycin has high purity.

Description

technical field [0001] The invention relates to the field of biopharmaceuticals, in particular to a production method of milbemycin. Background technique [0002] Milbemycin is a mixture with hexadecanolide structure isolated from Milbemycin fermentation broth. As a new biological pesticide, milbemycin is broad-spectrum, highly efficient and low-toxic, and is one of the most active insecticides; at the same time, milbemycin is also the direct raw material for the synthesis of milbemycin, which is a The novel synthetic macrolide anthelmintic drug has good effects on controlling and preventing most parasitic diseases. [0003] At present, the production method of milbemycin is to filter out the bacteria residue from the fermentation broth, and then use acetone or ethanol to extract the bacteria residue to obtain a milbemycin extract; Dilute the diluted milbemycin extract (column solution) with resin, and elute with ethanol-water or acetone-water to obtain an eluate; concentr...

Claims

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Application Information

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IPC IPC(8): C07D493/22
CPCC07D493/22
Inventor 刘小刚黄志强梁倍陈明渝王为民
Owner LIVZON GROUP FUZHOU FUXING PHARMACEUTICAL CO LTD
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