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Extraction method for spinosad

A spinosyn and extraction method technology, applied in chemical instruments and methods, organic chemistry, sugar derivatives, etc., can solve the problems of long production cycle, poor product crystal form, high energy consumption, etc. Low, high purity effect

Active Publication Date: 2020-05-19
HUBEI RUIHAO ANKE MEDICINE TECH DEV CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But because what this technique adopts is the direct solvent extraction method of fermented liquid, need larger solvent extraction (1.5 times of fermented liquid volume) just can guarantee the leaching yield of spinosad, and after leaching is finished, also need to further concentrate and remove high Polar solvent with dielectric constant, the process has problems such as large amount of solvent used, large energy consumption required to remove solvent, long production cycle (fermentation liquid needs to be stirred and extracted for 4 to 20 hours); This process only adopts the method of washing with dilute lye to fail to improve the internal quality of spinosad preferably, and most of the pigments of the powder and the impurities precipitated together by alkali adjustment cannot be eradicated, and the crystal form of the product is relatively poor (because the alkali adjustment precipitates crystallization faster rate)

Method used

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  • Extraction method for spinosad
  • Extraction method for spinosad
  • Extraction method for spinosad

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] 1.1 Extract spinosad from Saccharopolyspora spinosa fermentation broth

[0056] 1) Take 20L of spinosad fermentation broth [batch number is A20180820, put in a 500L fermentation tank] with a potency of 2.0g / L, add 2M NaOH solution to adjust the pH to 9.0, stir for 10 minutes, add 400g of perlite, and continue stirring 30 minutes;

[0057] figure 2 It is the HPLC detection spectrum of the spinosyn fermentation broth sample; the following table 1 is the data of the HPLC detection spectrum.

[0058] Table 1

[0059]

[0060] 2) Then filter with a plate frame, wash with water until the color is lighter, stop filtering, and obtain 3.9 kg of filter cake;

[0061] 3) The filter cake was stirred and leached with 25L methanol-water (methanol to water volume ratio: 4:1) solution for 5 hours, and filtered to obtain 26L of the extract;

[0062] 4) Pass the extract solution through 1.5L strong basic anion resin (A850) for decolorization, collect the effluent, and after pas...

Embodiment 2

[0081] 2.1 Extraction of spinosyn from Saccharopolyspora spinosa fermentation broth

[0082] 1) Take 20L of spinosad fermentation broth [batch number is A20180820, taken from 500L fermenter culture fluid], the potency is 2.0g / L, add 2M NaOH solution to adjust the pH to 8.5, stir for 10 minutes, add 300g of perlite, continue Stir for 30 minutes;

[0083] 2) Then filter with a plate frame, wash with water until the color is lighter, stop filtering, and obtain 3.8kg of filter cake;

[0084] 3) The filter cake was stirred and leached with 30.4L methanol-water (methanol to water volume ratio: 2:1) solution for 5 hours, and filtered to obtain 31L of leaching solution;

[0085] 4) Pass the extract solution through 1.5L strong basic anion resin (A850) for decolorization, collect the effluent, and after passing through the column, use 3L methanol-water solution of the same concentration to elute the spinosad remaining on the column. The decolorized solution was concentrated in vacu...

Embodiment 3

[0098] 3.1 Extraction of spinosads from Saccharopolyspora spinosa fermentation broth

[0099] 1) Take 20L of spinosad fermentation broth [batch number is A20180820, taken from a 500L fermenter culture broth], the potency is 2.0g / L, add 2M NaOH solution to adjust the pH to 9.0, stir for 10 minutes, add 400g of perlite, continue Stir for 30 minutes;

[0100] 2) Then filter with a plate frame, wash with water until the color is lighter, stop filtering, and obtain 4.2kg of filter cake;

[0101] 3) The filter cake was stirred and leached with 25.6L methanol-water (methanol to water volume ratio: 5:1) solution for 3 hours, and filtered to obtain 26.5L of leaching solution;

[0102] 4) Pass the extract solution through 2.5L strong basic anion resin (201×7) for decolorization, collect the effluent, and after passing through the column, use 3L methanol-water solution of the same concentration to elute the spinosad remaining on the column. The decolorized solution was vacuum-concent...

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Abstract

The invention provides an extraction method for spinosad. The method includes the following steps: 1) adjusting the pH of a fermentation liquid to 8.5 to 9.5 to obtain a pre-treated fermentation liquid; 2) filtering the obtained pre-treated fermentation liquid and collecting the filter cake; 3) performing extraction on the obtained filter cake under stirring by using a methanol-aqueous solution, and performing filtration to obtain an extract liquid; 4) performing treatment on the obtained extract liquid by using strong-base anion resin for decolorization, and performing concentration until nomethanol flows out to obtain a decolorized concentrated liquid; 5) adding a non-water-insoluble organic solvent into the obtained decolorized concentrated liquid, performing extraction, and collectinga supported organic phase; 6) adding acidic water into the obtained supported organic phase, performing back extraction, and collecting a back-extracted phase; and 7) adjusting pH of the obtained back-extracted phase to 9.0-10.0 under stirring to make spinosad precipitated in the form of a crystal, performing filtration, and performing drying to obtain the spinosad powder. The purity of the product finally obtained by using the method provided by the invention is >=99.5%, and is far higher than a level which a method in the prior art can achieve.

Description

technical field [0001] The invention belongs to the technical field of pharmacy, relates to a method for extracting spinosyns, and more specifically relates to a method for extracting spinosyns from fermentation liquid of Saccharopolyspora spinosa. The invention further provides the obtained spinosyns Crude refined method. Background technique [0002] Spinosyn (Spinosad) is a macrolide compound produced by the soil actinomycete Saccharopolyspora spinosa through aerobic fermentation, and its main active ingredient is Spinosyn A (accounting for about 80-90 %) and Spinosyn D (about 10-20%). [0003] [0004] Spinosyn A: R=H; Spinosyn D: R=CH 3 [0005] Spinosyn structural formula [0006] Spinosad is a new type of broad-spectrum biopesticide with contact and ingestion toxicity. It is a microbial biopesticide with high efficiency, rapidity and low toxicity. Currently, there are reports on the extraction and separation of spinosads mainly including adsorption method and ...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/06
CPCC07H17/08C07H1/06
Inventor 罗汾李小兵赵光友
Owner HUBEI RUIHAO ANKE MEDICINE TECH DEV CO LTD
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