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Method for preparing echinocandin B

An Echinococcus Kangding and Kangding technology, applied in the direction of peptides, etc., can solve the problems of high column pressure, difficulty in scaling up the preparation process, and poor removal of pigments, etc., and achieve the effect of simple process and low cost

Inactive Publication Date: 2012-07-04
SHANGHAI INST OF PHARMA IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its main disadvantage is that the pressure of passing through the column is too high, and the preparation process is difficult to scale up; and it cannot remove the pigment in the upstream fermentation broth well

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Embodiment 1,2,3 investigate the influence of the fermented liquid of different pH on separation process

[0048] Example 1:

[0049] Take 500ml of Echinococcus Kangding B fermentation broth, the purity is 3.1%, and the unit is 647ug / ml, adjust the pH of the fermentation broth to 2.0 and let it stand for a while, discard the supernatant after high-speed centrifugation, and use 1.5 times the mycelia Echinocandin B was extracted by immersion in methanol, and the mycelium was removed by filtration. After the methanol was evaporated to dryness, Echinocandin B was extracted with the same volume of n-butanol, and the insoluble matter was removed by filtration. The purity was 8.0 %.

[0050] Install a HP20 resin column with a height of about 20 cm and a diameter of about 4 cm, evaporate Echinococdin B to dryness and dissolve it in 3:1 methanol water, and pass through the column at a flow rate of 10 ml / min. Echinococtant B is completely adsorbed on On the column, the column w...

Embodiment 2

[0053] Example 2: Optimal pH

[0054] Take 500ml of Echinococcus Kangding B fermentation broth, the purity is 3.1%, and the unit is 647ug / ml, adjust the pH of the fermentation broth to 3.0 and let it stand for a while, discard the supernatant after high-speed centrifugation, and use 1.5 times the mycelia Echinocandin B was extracted by immersion in methanol, and the mycelium was removed by filtration. After the methanol was evaporated to dryness, Echinocandin B was extracted with the same volume of n-butanol, and the insoluble matter was removed by filtration. The purity was 8.9 %.

[0055] Install a HP20 resin column with a height of about 20 cm and a diameter of about 4 cm, evaporate Echinococdin B to dryness and dissolve it in 3:1 methanol water, and pass through the column at a flow rate of 10 ml / min. Echinococtant B is completely adsorbed on On the column, the column was eluted with 9:1 methanol water, and the part with higher purity in the eluate was distributed and col...

Embodiment 3

[0059] Take Echinococcus Kangding B fermentation liquid 500ml, its purity is 3.1%, the unit is 647ug / ml, adjust the pH of the fermentation liquid to 4.0 and let it stand for a period of time, discard the supernatant after high-speed centrifugation, and use 1.5 times the mycelium Echinocandin B was extracted by immersion in methanol, and the mycelium was removed by filtration. After the methanol was evaporated to dryness, Echinocandin B was extracted with the same volume of n-butanol, and the insoluble matter was removed by filtration. The purity was 7.9 %.

[0060] Install a HP20 resin column with a height of about 20 cm and a diameter of about 4 cm, evaporate Echinococdin B to dryness and dissolve it in 3:1 methanol water, and pass through the column at a flow rate of 10 ml / min. Echinococtant B is completely adsorbed on On the column, the column was eluted with 9:1 methanol water, and the part with higher purity in the eluate was distributed and collected. It was detected tha...

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Abstract

The invention discloses a method for preparing echinocandin B. The method comprises the following steps of: a) centrifuging the fermentation liquid of echinocandin B, taking mycelium, leaching the echinocandin B in the mycelium with a first solvent and filtering and removing the mycelium; b) distilling the solvent in the first solvent leaching solution of echinocandin B to dryness, soaking with asecond solvent and filtering and removing the insoluble substances; c) distilling the second solvent soak solution of echinocandin B to dryness and then dissolving in the first solvent, utilizing macroporous absorption resin, performing eluting with the first solvent and collecting the part with higher purity; d) distilling the collected solution of echinocandin B to dryness and then dissolving in the second solvent, utilizing an alumina column, performing eluting with the first solvent and collecting eluent; e) distilling the eluent of echinocandin B to dryness and then dissolving in the first solvent, utilizing inverse resin, performing eluting with the first solvent and then collecting the part with higher purity; and f) distilling the collected solution of echinocandin B to dryness and then dissolving in the first solvent, adding in a small amount of water by dripping to achieve the purpose of separation by crystallization after supersaturation, and preparing the echinocandin B. The method for preparing the echinocandin B not only can well remove the pigment, but also is suitable for the large-scale industrial production and has good commercial value; and the method leads the final purity of the echinocandin B to be improved by more than 95 percent.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and in particular relates to a method for preparing Echinocandin B, a precursor of Anifungin. Background technique [0002] Since the 1970s, in the course of clinical treatment, fungal infection diseases and the death rate caused by uncontrollable fungal infections have gradually increased, which is related to the widespread use of drugs that damage the human immune system and the extensive use of broad-spectrum antibacterial drugs. direct relationship. Also, associated with clinical use of internal implants and infection with chronic immunosuppressive viruses like AIDS. Therefore, it is very important to research and develop safe, new and effective antifungal drugs. As we all know, fungal cells have cell walls, mammalian cells do not have cell walls. Therefore, the cell wall of fungi should be used as the target of new antifungal drugs. Echinocandines are drugs that act on the cell wall of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07K7/56
Inventor 李继安卢亮颜晨晨林惠敏
Owner SHANGHAI INST OF PHARMA IND CO LTD