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A kind of extraction and purification method of fumagillin

A technology of fumagillin and purification method, applied in the direction of organic chemistry and the like, can solve the problems of complex operation steps, high cost, multiple impurities, etc., and achieve the effects of simple process operation, low cost and high purity

Active Publication Date: 2020-07-31
ZHEJIANG HISUN PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Wherein one-step resin chromatography can obtain the crystal of 81.2% chromatographic purity, needs two-step resin chromatography and just can obtain 95.2% chromatographic purity crystal, and operation procedure is complicated; Simultaneously, the water solubility of fumagillin is very poor, very sensitive to light and heat Unstable, long chromatographic cycle, easy to produce more impurities; macroporous adsorption resin needs to be eluted with aqueous solvent, and requires more eluent, and the cost is higher; in summary, the above method is not conducive to fumagillin large-scale industrial production of
[0007] In addition, all the above processes are for the extraction of extracellular fumagillin, without considering the extraction of intracellular fumagillin
[0008] In summary, the existing technology can not well meet the needs of large-scale industrial production of fumagillin

Method used

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  • A kind of extraction and purification method of fumagillin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] The preparation of embodiment 1 fumagillin fermented liquid

[0043] The strain used in the fermentation culture in the examples of the present invention is a new fumagillin-producing strain, which is Penicillium sp. HS-NF-684Z, and its preservation number is CGMCC No. 14144.

[0044] The microbial strain of Penicillium HS-NF-684Z was preserved on July 24, 2017 in the General Microbiology Center of the China Committee for the Collection of Microbial Strains (Address: No. 3, Yard 1, Beichen West Road, Chaoyang District, Beijing, Microbiological Research, Chinese Academy of Sciences Institute), the preservation number is CGMCC No.14144, the classification name is Penicillium sp., and it is registered in the register to prove its survival.

[0045] The fumagillin fermented liquid culture process of the present invention is as follows:

[0046] (1) Preparation and cultivation of slant colonies

[0047] Potato glucose agar medium (g / L) was used as the slant medium: potato ...

Embodiment 2

[0055] Example 2 Fumagillin extraction and purification (carried out under dark)

[0056] Step a): get 30L of fumagillin fermented liquid (obtained according to the method described in Example 1), the total titer of fumagillin in the cell and extracellular is 1010mg / L (extracellular fumagillin effect valence is 216mg / L), add 45L MTBE (methyl tert-butyl ether), stir for 1h, let stand for 8h, separate liquid, collect MTBE extract phase 42L, take MTBE extract phase and analyze by HPLC, fumagillin concentration is 584.5 mg / L, the extraction yield was 81.0%;

[0057] Step b): Concentrate the MTBE extract phase obtained in step a) to 1.1 L at a concentration temperature of 30°C, then lower the temperature to 0°C, stir for 8 hours, and filter to obtain 50.0 g of fumagillin wet solid;

[0058] Step c): Dissolve the fumagillin wet solid obtained in step b) with 200ml of a mixed solvent of dichloromethane and methanol (the volume ratio of dichloromethane to methanol is 1:1), and filter...

Embodiment 3

[0060] Example 3 Fumagillin extraction and purification (carried out under dark)

[0061] Step a): get 30L of fumagillin fermented liquid (obtained according to the method described in Example 1), the total titer of fumagillin in the cell and extracellular is 1032mg / L (extracellular fumagillin effect valence is 180mg / L), add 90L ETBE (ethyl tert-butyl ether), stir for 5h, let stand for 10h, separate liquid, collect ETBE extract phase 84L, get ETBE extract phase and analyze by HPLC, fumagillin concentration is 310.2 mg / L, the extraction yield was 84.2%;

[0062] Step b): Concentrate the ETBE extract phase obtained in step a) to 2.8L, the concentration temperature is 30°C, then lower the temperature to 15°C, stir for 12h, and filter to obtain 52.6g of fumagillin wet solid;

[0063] Step c): Dissolve the fumagillin wet solid obtained in step b) with 420ml of a mixed solvent of dichloromethane and methanol (the volume ratio of dichloromethane to methanol is 5:1), and filter to ob...

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Abstract

Provided is a fumagillin extraction and purification method, which comprises the steps of extraction with a methyl t-butyl ether (MTBE) or ethyl t-butyl ether (ETBE) fermentation liquid, MTBE or ETBE precipitation, crystallization and purification, etc. The method is simple to operate, has a high yield, a low cost, can be industrialized on a large scale, and has great a significance for the industrialized production of fumagillin and the later development of a fumagillin derivative.

Description

technical field [0001] The present invention relates to the field of pharmacy. Specifically, the present invention relates to a method for extracting and purifying fumagillin. Background technique [0002] Fumagillin (Fumagillin, formula I) is a metabolite with various biological activities isolated from the fermentation broth of Aspergillus Fumigatus for the first time. Initially, fumagillin was used to kill microsporidian parasites in honey bees, but was later found to be useful in the treatment of microsporidiosis and / or cryptosporidiosis caused by intestinal infections in humans, which are critical for immune Deficient patients are quite deadly. In addition, fumagillin is almost insoluble in water, and is easily degraded by light, which greatly affects its bioavailability. However, researchers have found that fumagillol and other derivatives are stable in nature and have better effects than fumagillin, while fumagillol and other related derivatives are prepared from f...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/16C07D301/32
CPCC07D301/32C07D303/16
Inventor 李建宋王继栋张辉姜南张延青钱娉婷邓爱文应灵萍滕云郑玲辉
Owner ZHEJIANG HISUN PHARMA CO LTD
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