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Method for preparing pneumocandin B0

A technology of neomycin and solvent, which is applied in the field of preparing nemocontin B0, a precursor of carpafungin, can solve the problems of cumbersome process, difficulty in removing pigments from fermentation broth, etc., and achieves a simple process, low cost and improved purity. Effect

Inactive Publication Date: 2010-03-03
SHANGHAI INST OF PHARMA IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] In order to solve the problem of preparing pneumocidine B in the prior art 0 It is difficult to remove the pigment in the fermented liquid by the process, and the whole process is relatively cumbersome technical problem. The present invention provides a method for preparing pneumocidine B 0 Simple method, this method can not only remove pneumocidine B well 0 Pigment in the medium, and can increase its purity to more than 96%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] nemocontin B 0 Fermentation broth 500ml, its purity is 8%, the unit is 683ug / 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, soak the mycelium with 1.5 times methanol to extract it Neomercantin B 0 , remove the mycelium by filtration, then evaporate the methanol to dryness, and use the same volume of n-butanol to leach pneumocidine B 0 , and filter out the insoluble matter therein, and detect that its purity is 14.7%.

[0057] Install an alumina column with a height of about 15 cm and a diameter of 3 cm. Neomercantin B 0 After the n-butanol leaching solution is evaporated to dryness, it is made into 4:1 methanol water and then passes through the alumina column at a faster flow rate, and then passes through the column with twice the column volume of methanol water in the same ratio, and collects all the effluents. Neomercontin B 0 The purity is 34.9%, and the pigment is basical...

Embodiment 2

[0061] nemocontin B 0 Fermentation broth 500ml, its purity is 13%, the unit is 596ug / ml, adjust the pH of the fermentation broth to 3.0 and let it stand for a period of time, discard the supernatant after high-speed centrifugation, soak the mycelium with 1.5 times methanol to extract it Neomercantin B 0 , remove the mycelium by filtration, then evaporate the methanol to dryness, and use the same volume of n-butanol to leach pneumocidine B 0 , Remove the insolubles therein by filtration, and detect that its purity is 16.9%.

[0062] Install an alumina column with a height of about 15 cm and a diameter of 3 cm. Neomercantin B 0 After the n-butanol leaching solution is evaporated to dryness, it is made into 4:1 methanol water and then passes through the alumina column at a faster flow rate, and then passes through the column with twice the column volume of methanol water in the same ratio, and collects all the effluents. Neomercontin B 0 The purity is 42.7%, and the pigment ...

Embodiment 3

[0066] nemocontin B 0 Fermentation broth 500ml, its purity is 13%, the unit is 596ug / ml, adjust the pH of the fermentation broth to 4.0 and let it stand for a period of time, discard the supernatant after high-speed centrifugation, soak the mycelium with 1.5 times methanol to extract it Neomercantin B 0 , remove the mycelium by filtration, then evaporate the methanol to dryness, and use the same volume of n-butanol to leach pneumocidine B 0 , Remove the insolubles therein by filtering, and detect that its purity is 14.8%.

[0067] Install an alumina column with a height of about 15 cm and a diameter of 3 cm. Neomercantin B 0 After the n-butanol leaching solution is evaporated to dryness, it is made into 4:1 methanol water and then passes through the alumina column at a faster flow rate, and then passes through the column with twice the column volume of methanol water in the same ratio, and collects all the effluents. Neomercontin B 0 The purity is 39.4%, and the pigment i...

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Abstract

The invention discloses a method for preparing pneumocandin B0. The method comprises the following steps of: a) centrifuging the fermentation liquid of echinocandin B0, taking mycelium, leaching the echinocandin B0 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 B0 to dryness, soaking with a second solvent and then filtering and removing the insoluble substances; c) distilling the second solvent soak solution of echinocandin B0 to dryness and then dissolving in the first solvent, andcollecting effluent liquid through overly acidic alumina column; d) distilling the collected solution of echinocandin B0 to dryness and then dissolving in the first solvent, utilizing adsorbent resin,performing eluting with the first solvent and then collecting the part with higher purity; e) distilling the collected solution of echinocandin B0 to dryness and then dissolving in the first solvent,utilizing inverse resin, performing eluting with the first solvent and collecting the part with higher purity; and f) distilling the collected solution of echinocandin B0 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 then preparing the echinocandin B0. The methodfor preparing the echinocandin B0 not only can well remove the pigment, but also leads the purity of the echinocandin B0 to be improved by more than 96 percent.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and in particular relates to a precursor pneumocontin B for preparing carpafungin 0 Methods. 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. Nemocontins are drugs that act on the cell wall of fu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K7/56
Inventor 李继安卢亮林惠敏刘笑芬
Owner SHANGHAI INST OF PHARMA IND
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