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A method for extracting and purifying milbemycin from fermentation broth

A technology of mirbemycin and fermentation broth, applied in the field of purification and extraction of biological pesticides, can solve problems such as mirbemycin that has not been seen yet, and achieve the effects of low requirements, mild conditions and high purity

Active Publication Date: 2018-11-20
CHONGQING DAXIN PHARMA +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is no patent research report on the extraction and purification of milbemycin from the fermentation broth

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  • A method for extracting and purifying milbemycin from fermentation broth

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Embodiment 1

[0042] Flocculation and filtration of milbemycin fermentation broth. Take 20L of milbemycin fermentation broth (milbemycin unit: 980 μg / mL) produced by Chongqing Daxin Pharmaceutical Co., Ltd., heat to 65°C, keep it warm for 40 minutes, and stir at the same time; add flocculant PAM 0.05% W / V , flocculate for 30 minutes; add 400g of perlite powder filter aid, and vacuum filter to obtain 1500g of wet mycelium residue.

Embodiment 2

[0044] Flocculation and filtration of milbemycin fermentation broth. Take 20L of milbemycin fermentation broth produced by Chongqing Daxin Pharmaceutical Co., Ltd. (milbemycin unit 1020 μg / mL), heat to 80°C, keep it warm for 30 minutes, and stir at the same time; add 1% polyaluminum chloride as a flocculant W / V, flocculate for 30 minutes; add 400g of perlite powder filter aid, and vacuum filter to obtain 1700g of wet mycelium residue.

Embodiment 3

[0046] Bacteria residue extraction: add 5L of butyl acetate to 1500g of wet mycelia residue obtained in Example 1, stir and extract at 28-30°C for 3.5 hours, filter and collect 4.1L of the extract; Extract the residue, stir and extract at 28-30°C for 2 hours, collect the extract by filtration, and combine and collect 9.2 L of the extract, which is the primary extract (milbemycin unit: 2002 μg / mL).

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Abstract

The invention discloses a method for extracting and purifying milbemycins from a fermentation liquid. The method comprises the following steps: flocculating and filtering a milbemycins fermentation liquid to obtain hypha residues; extracting the hypha residues by using a water-insoluble solvent, performing acid washing, concentration and alkali treatment on the extracting liquid sequentially, and performing extraction for the second time; performing acid washing and cooling precipitation, filtering and performing silica gel column chromatography on the filtrate; performing derivatization treatment on desorption liquid, performing silica gel column chromatography for the second time, and performing crystallization and separation to obtain milbemycins derivatives; hydrolyzing, extracting, concentrating, crystallizing and drying the derivatives to obtain milbemycins with milbemycins A3 content and milbemycins A4 content being more than 80 percent. The method is low in requirements on production equipment, mild in condition, simple and easy to operate, high in purity of the obtained milbemycins, suitable for large-scale production and remarkable in economic benefit.

Description

technical field [0001] The invention relates to a method for extracting and purifying biological pesticides, in particular to a method for extracting milbemycin from a fermented liquid and then purifying it to obtain high-purity milbemycin. Background technique [0002] Milbemycins (milbemycins) was isolated from Streptomyceshygroscopicussugsp, aureolacrimosus fermentation broth by Aoki et al. of Sankyo Company in Japan in 1967. It is an antibiotic with a mixture of sixteen ring lactones. Milbemycin has a high control effect on various mites. Most of the 20 components of the natural product have broad-spectrum control activities against agricultural pests, such as aphids, mites, yellow-brown tent caterpillars, intestinal parasites and other parasites that harm crops and livestock. The drug has a strong effect on pests, less dosage, is safe for humans and animals, does not pollute the environment, only kills insects, does not harm natural enemies, and is not easy to produce ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/22
CPCC07D493/22
Inventor 李华德张洪兰康正磊
Owner CHONGQING DAXIN PHARMA
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