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Preparation method for high-purity micafungin precursor compound

The technology of a precursor compound, micafungin, is applied in the preparation method of peptides, chemical instruments and methods, organic chemistry, etc., and can solve the problems that have not been reported in the extraction and purification, and achieve quality control, high sample purity, The effect of simple process

Active Publication Date: 2013-03-06
NCPC NEW DRUG RES & DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Journal of bioscience and bioengineering, The journal of antibiotics, and Bioorganic&medicinal chemistry letters have a small number of documents related to FR901379, all of which are reports on microbial cultivation and structural modification, and no reports on extraction and purification

Method used

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  • Preparation method for high-purity micafungin precursor compound
  • Preparation method for high-purity micafungin precursor compound
  • Preparation method for high-purity micafungin precursor compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Take 5.0L of micafungin precursor compound FR901379 fermentation broth, the fermentation unit is 1320μg / mL, and suction-filter to obtain 1.1kg of solid-state fermentation culture, add 1.25L of 95% ethanol, stir and extract at room temperature for 60min, suction-filter, and collect the filtrate. Add 1 L of 95% ethanol to the filter cake, stir at room temperature for 30 minutes, vacuum filter, and combine the filtrate (see attached figure 1) , add water to adjust the ethanol concentration to 30%, adsorb with 800mL D312 resin, wash 2400mL with 50% ethanol, elute with 80% ethanol until the elution of FR901379 is completed, and concentrate the 80% ethanol eluate to ethanol under reduced pressure at 40°C The concentration was less than 2%, cooled to 20°C, suction filtered, and vacuum-dried at 40°C to obtain 7.16g of crude extract of FR901379, which was dry-loaded on a 500mL silica gel column and eluted with ethyl acetate-petroleum ether 7;3, HPLC Detection, combined area per...

Embodiment 2

[0035] Take 10.0L of micafungin precursor compound FR901379 fermentation broth, the fermentation unit is 1140μg / mL, and filter to obtain 2.1kg of solid fermentation broth culture, add 3.0L of 95% ethanol, stir and extract at room temperature for 90min, filter with suction, and collect the filtrate (with attached Figure 1 peak shape similar), add 2.0L concentration of 95% ethanol to the filter cake, vacuum filter after stirring at room temperature for 60min, combine the filtrate, add water to adjust the concentration of ethanol to 35%, adsorb with 1200mLHZ-816 resin, wash 1200mL with 50% concentration of methanol , eluted with 85% concentration of methanol until the elution of FR901379 is completed, the 85% methanol eluate is concentrated under reduced pressure at 40°C to a methanol concentration of less than 2%, cooled to 20°C, suction filtered, and vacuum-dried at 40°C to obtain rice 12.63 g of crude extract of cafungin precursor compound FR901379. Load the sample on a 700m...

Embodiment 3

[0037]Take 8.0L of micafungin precursor compound FR901379 fermentation broth, the fermentation unit is 1260μg / mL, and suction filter to obtain 1.4kg of solid fermentation broth culture, add methanol 4L, stir and extract at room temperature for 30min, suction filtration, collect the filtrate, filter cake Add 2L of methanol, stir at room temperature for 30min, then vacuum filter, and combine the filtrate (with the attached Figure 1 peak similar in shape), add water to adjust the concentration of methanol to 40%, adsorb with 1200mL D312 resin, wash 2000mL with 50% concentration of methanol, and elute with 80% concentration of methanol until the elution of FR901379 is completed. Concentrate until the concentration of methanol is less than 2%, cool to 20°C, filter with suction, and dry under vacuum at 40°C to obtain 9.45 g of crude extract of FR901379. Load the sample on a 500mL silica gel column by dry method, elute with acetone-petroleum ether 6;4, detect by HPLC, combine the pa...

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PUM

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Abstract

The invention discloses a preparation method for a micafungin precursor compound by using a Coleophoma sp. fermentation culture. The method comprises the following steps: carrying out filtration, digestion, resin adsorption, desorption, condensation and the like on the Coleophoma sp. fermentation culture so as to obtain a crude extract of FR901379; and carrying out further purification on the crude extract of the FR901379 by using silica gel chromatography so as to obtain a micafungin precursor compound FR901379 product with high purity. The invention has the following advantages: resin adsorption and silica gel chromatography are used to extract and separate the FR901379 in the method to prepare the micafungin precursor compound FR901379 with high purity, and the method is simple and feasible and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of industrial microorganisms, and in particular relates to a preparation method of a high-purity micafungin precursor compound FR901379. Background technique [0002] In recent years, with the extensive application of broad-spectrum antibacterial drugs and immunosuppressants, tumor chemotherapy, organ transplantation, and the spread of AIDS, the number of people with suppressed immune systems has increased, and the incidence of deep fungal infections has begun to show a clear upward trend. , and with the application of antifungal drugs, the drug resistance of fungi is getting stronger and stronger, making the application of antifungal drugs have a trend of rapid increase. Therefore, anti-deep fungal infection drugs have become one of the research hotspots of anti-infective drugs and have attracted people's attention day by day. [0003] Echinocandin is a new type of antifungal drug, which has a significantl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K7/56C07K1/22C07K1/16
Inventor 李宁张雪霞李晓露王海燕林毅张金娟林旸张丽任风芝成晓迅陈书红张艳哲张艳立李岳段宝玲
Owner NCPC NEW DRUG RES & DEV
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