Method for extracting pleocidin from saccharopolyspora spinosa fermentation liquor

A technology of Saccharopolyspora spinosa and spinosad, which is applied in the field of spinosad extraction, can solve the problems of serious environmental pollution, high difficulty in wastewater treatment, and large usage, so as to achieve safe operation, reduce the difficulty of wastewater treatment, and reduce the The effect of usage

Active Publication Date: 2014-09-24
HUNAN HAILI CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The purpose of the present invention is to overcome the disadvantages such as large amount of organic solvent used in the prior art, high difficulty in wastewater trea...

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  • Method for extracting pleocidin from saccharopolyspora spinosa fermentation liquor
  • Method for extracting pleocidin from saccharopolyspora spinosa fermentation liquor

Examples

Experimental program
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Effect test

Embodiment 1

[0024] ①Add 1000mL of fermentation broth (containing 0.56g of spinosad) to the alkalization kettle, adjust the pH of the fermentation broth to 9 with 30% NaOH solution, stir at room temperature for 30 minutes and centrifuge to obtain 52g of solid; ②Add to the water phase after one centrifugation 50g of bentonite, stirred at room temperature for 30min, centrifuged to obtain 56g of solid, and the second centrifuge liquid was sent to waste water for treatment; ③Combine the solid after the first and second centrifugation, and dry it under vacuum (1.33kPa) at 50°C for 5h to obtain 93g of dry solid; ④Use cable 186g n-pentane was added, refluxed for 3h; ⑤ under reduced pressure (1.33kPa) precipitation, adding 5g n-pentane recrystallization, to get 0.47g spinosad product, content 90.0% (liquid chromatography, external standard; Component A84.7%, component D5.3%), yield 76.2%.

Embodiment 2

[0026] ① Add 1000mL of fermentation broth (containing 0.56g of spinosad) to the alkalization kettle, adjust the pH of the fermentation broth to 8 with 20% NaOH solution, stir at room temperature for 15 minutes and then centrifuge to obtain 52g of solid; ② Add to the water phase after one centrifugation 50g of activated carbon was centrifuged at 5°C for 60min to obtain 58g of solid, and the second centrifuge was sent to waste water for treatment; ③Combine the solid after the first and second centrifugation, and dry it under vacuum (1.33kPa) at 30°C for 8h to obtain 92g of dry solid; ④Use Soxhlet extraction method, add 92g methanol, reflux 8h; ⑤ desolvation under reduced pressure (1.33kPa), add 5g cyclohexane recrystallization, get 0.71g spinosad product, content 75.0% (liquid chromatography, external standard; Component A70.7%, component D4.3%), yield 95.0%.

Embodiment 3

[0028] ①Add 1000mL of fermentation broth (containing 0.56g of spinosad) to the alkalization kettle, adjust the pH of the fermentation broth to 10 with 50% NaOH solution, stir at room temperature for 15 minutes and then centrifuge to obtain 53g of solid; ②Add to the water phase after one centrifugation 50g of macroporous resin was centrifuged at 50°C for 15 minutes to obtain 57g of solid, and the second centrifugal liquid was sent to waste water for treatment; ③Combine the solid after the first and second centrifugation, and dry it under vacuum (1.33kPa) at 80°C for 1 hour to obtain 91g of dry solid; 4. Adopt Soxhlet extraction method, add 455g ethanol, reflux 1h; 5.Desolvation under reduced pressure (1.33kPa), add 5g n-hexane recrystallization, get 0.47g spinosad product, content 84.0% (liquid chromatography, external standard; Component A79.1%, component D4.9%), yield 70.0%.

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Abstract

The invention relates to a method for extracting pleocidin from saccharopolyspora spinosa fermentation liquor. The method comprises the following steps: (1), pre-treating saccharopolyspora spinosa fermentation liquor and carrying out solid-liquid separation; (2), adsorbing centrifuged organic substances in a water phase by an adsorbent; (3), combining solids which are centrifuged and separated for the first time and the second time, and drying in vacuum; (4), extracting pleocidin from solids; and (5), recrystallizing by using a solvent to obtain a pleocidin product, decompressing and desolventizing. According to the method disclosed by the invention, a polar solvent is not needed to be added for extracting during pre-treatment, so that usage amount of an organic solvent is greatly reduced, pollution is reduced, cost is lowered, a centrifugal method can be adopted, operation is safe and separating effect is good; moreover, the adsorbent is added into the water phase for adsorbing organic substances in water, so that COD (chemical oxygen demand) in wastewater is greatly lowered, wastewater treating difficulty is reduced, the yield of the obtained product pleocidin is higher, and a total yield is 70%-95%; after the product is purified, the pleocidin content with mass content of 75%-93.2% is higher.

Description

technical field [0001] The invention relates to a process for extracting antibiotics from fermented liquid, in particular to a new process for extracting spinosads from fermented liquid of Saccharopolyspora spinosa. Background technique [0002] Spinosad is an intracellular secondary metabolite produced by the soil actinomycete Saccharopolyspora spinosa after aerobic fermentation, and it belongs to macrolide compounds. So far, more than 20 spinosyn components and more than 800 synthetic and semi-synthetic spinosyn analogues have been isolated from S. spinosa fermentation broth. Among the components extracted from natural spinosad, the two most active components are the mixture of Spinosyn A and D, which is called Spinosad, and its chemical structure is shown below. [0003] [0004] Spinosad can effectively control pests of Lepidoptera, Diptera and Thysanoptera, and at the same time, it can effectively control some specific pests of Coleoptera, Orthoptera, Hymenoptera, I...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/06
Inventor 罗先福曾雪云王燕刘世明陈明臧阳陵
Owner HUNAN HAILI CHEM IND
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