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A method for extracting and purifying spinosad from fermentation broth

A spinosad, fermentation broth technology, applied in chemical instruments and methods, botanical equipment and methods, biocides, etc., can solve the problems of large solvent usage, safety risks, spinosad damage, long cycle and other problems. Reduced safety risks, less solvent usage, low cost effects

Active Publication Date: 2021-08-27
NEW FOUNDER HLDG DEV LLC +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the prior art, the extraction method of spinosad mostly adopts the addition of filter aid, high temperature heating or centrifugal pretreatment of the fermented liquid (such as the Chinese patents with publication numbers CN107474088A, CN109628530A and CN101906124B), or adding organic solvents such as acetone Extraction, or the separation and purification of spinosyn by conventional techniques such as macroporous resin adsorption under the solvent-containing situation (as the Chinese patents with publication numbers CN107474088A, CN109628530A, CN109929004N and CN104059117A), in the above method, using heating will cause damage to spinosyn Destruction, using solvent extraction and resin separation methods, there are safety risks due to the excessive use of solvents, and the cycle is long and the cost is high

Method used

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Examples

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Embodiment 1

[0044] The present embodiment provides a method for extracting and purifying spinosad from fermentation broth, the specific process is as follows:

[0045] (1) Get 30L of spinosad fermented liquid, spinosad unit 2500ug / ml, add ammonia water to adjust its pH to 8.5, plate and frame filter after complete precipitation, wash with water, air-dry, obtain filter residue;

[0046] (2) Dissolve the filter residue in 7.5 times the volume of water, add hydrochloric acid to adjust the pH to 2.5, filter through a ceramic membrane with a pore size of 0.01-0.1 μm, and wash with 4 times the volume of spinosad fermentation broth, collect the filtrate and use The nanofiltration membrane with a pore size of 100-200Da is concentrated to a volume of 0.4 times the volume of the spinosad fermentation broth to obtain a concentrated solution. At the same time, the total yield of plate and frame filtration and ceramic membrane filtration is 83%;

[0047] (3) Add butyl acetate to the concentrated solut...

Embodiment 2

[0052] The present embodiment provides a method for extracting and purifying spinosad from fermentation broth, the specific process is as follows:

[0053] (1) Get 30L of spinosad fermented liquid, the spinosad unit is 2490ug / ml, add ammonia water to adjust its pH to 9.0, filter the plate and frame after complete precipitation, wash with water, and air-dry to obtain the filter residue;

[0054] (2) Dissolve the filter residue in 6 times the volume of water, add hydrochloric acid to adjust the pH to 3.0, filter through a ceramic membrane with a pore size of 0.01-0.1 μm, and wash with 3.5 times the volume of spinosad fermentation liquid, collect the filtrate and use The nanofiltration membrane with a pore size of 100-200Da is concentrated to a volume of 0.45 times the volume of the spinosad fermentation broth to obtain a concentrated solution. At the same time, the total yield of plate and frame filtration and ceramic membrane filtration is 87%;

[0055] (3) Add ethyl acetate to...

Embodiment 3

[0060] The present embodiment provides a method for extracting and purifying spinosad from fermentation broth, the specific process is as follows:

[0061] (1) Get 30L of spinosad fermented liquid, the spinosad unit is 2680ug / ml, add ammonia water to adjust its pH to 10.0, filter the plate and frame after complete precipitation, wash with water, and air-dry to obtain the filter residue;

[0062] (2) Dissolve the filter residue in 7.5 times the volume of water, add phosphoric acid to adjust the pH to 3.0, filter through a ceramic membrane with a pore size of 0.01-0.1 μm and wash with 4.5 times the volume of spinosad fermentation broth, collect the filtrate and use The nanofiltration membrane with a pore size of 100-200Da is concentrated to a volume of 0.38 times the volume of the spinosad fermentation broth to obtain a concentrated solution. At the same time, the total yield of plate and frame filtration and ceramic membrane filtration is 82.7%;

[0063] (3) Add butyl acetate t...

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Abstract

The invention discloses a method for extracting and purifying spinosad from a fermentation broth, comprising: adding alkali to the spinosad fermentation broth to adjust the pH to be greater than 8, and separating solid and liquid after precipitation to obtain a filter residue; dissolving the filter residue in water , add acid to adjust the pH to less than 5, concentrate after filtration to obtain a concentrated solution; add an organic solvent to the concentrated solution for extraction treatment, add activated carbon to decolorize after collecting the organic layer, and obtain an extraction decolorization solution; add acid solution to the extraction decolorization solution. Extraction treatment, after collecting the water layer, add activated carbon for decolorization to obtain a back-extraction decolorization liquid; add alkali to the back-extraction decolorization liquid for crystallization, and separate and obtain the crude spinosad. The method of the present invention comprehensively adopts plate and frame filtration, ceramic membrane filtration, extraction, washing, decolorization, back extraction, decolorization and crystallization technology, and has short process cycle, no heating, less use of solvent, high impurity removal efficiency, simple process operation and low cost , suitable for industrial production of spinosad.

Description

technical field [0001] The invention belongs to the technical field of biological medicine purification, and in particular relates to a method for extracting and purifying spinosad from fermentation broth. Background technique [0002] Spinosyn, also known as spinosad (Spinosad), is a kind of macrolide pollution-free and high-efficiency biopesticide extracted from the fermentation broth of Saccharopolyspora spinosa. Spinosyn producing parent strain soil actinomycete Saccharopolyspora spinosa Metrz & Yao originally isolated from an abandoned winery in the Caribbean; investigator at Dow AgroSciences (now Dow AgroSciences) It was found that the bacterium can produce compounds with very high insecticidal activity, and the practical product is a mixture of spinosyn A and spinosyn D, so it is called Spinosad. [0003] Spinosad has a novel mode of action, which can continuously activate the target insect acetylcholine nicotinic receptor, but its binding site is different from that...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/08C07H1/06A01N43/22A01P7/04
CPCA01N43/22C07H1/06C07H17/08
Inventor 赵燕封维张葵
Owner NEW FOUNDER HLDG DEV LLC
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