Method for purifying echinocandin B parent nucleus

A technology of echinocandin and parent nucleus, which is applied in the field of drug synthesis to achieve the effects of easy recycling and reuse, saving time and cost

Active Publication Date: 2018-03-09
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are three types of echinocandin antibiotics: B, C and D, among which echinocandin B (ECB for short) is the most important type, but due to the presence of acyl side chains, it has certain hemolytic toxicity.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take 100L of echinocandin B nuclei conversion solution, microfiltration to obtain the liquid phase, wash the solid phase with water until the conductivity of the effluent is less than 100μs, and obtain 250L of the liquid. Concentrate by microfiltration to an echinocandin B nucleus concentration of 20g / L.

[0030] The pH value was adjusted to 3.5 with hydrochloric acid, and acetone was added to precipitate the echinocandin B nucleus. Centrifuge at 3000 rpm for 15 min with a 120-mesh filter cloth. The crystals of echinocandin B core were collected from the filter cloth, put into a fume hood, and blown with sterile air overnight to obtain a dry solid powder.

[0031] The purity of echinocandin B mother nucleus is 98.3% and the yield is 72% through high-pressure liquid phase detection.

Embodiment 2

[0033] Take 100L of echinocandin B nuclei conversion solution, microfiltration to obtain the liquid phase, wash the solid phase with water until the conductivity of the effluent is less than 100μs, and obtain 250L of the liquid. Concentrate by microfiltration to an echinocandin B nucleus concentration of 35g / L.

[0034] The pH value was adjusted to 4.0 with hydrochloric acid, and acetone was added to precipitate the echinocandin B nucleus. Centrifuge at 3000 rpm for 15 min with a 120-mesh filter cloth. The crystals of echinocandin B core were collected from the filter cloth, put into a fume hood, and blown with sterile air overnight to obtain a dry solid powder.

[0035] The purity of echinocandin B mother nucleus was 98.2% and the yield was 82% through high-pressure liquid phase detection.

Embodiment 3

[0037] Take 100L of echinocandin B nuclei conversion solution, microfiltration to obtain the liquid phase, wash the solid phase with water until the conductivity of the effluent is less than 100μs, and obtain 260L of liquid. Concentrate by microfiltration to an echinocandin B nucleus concentration of 30g / L.

[0038] The pH value was adjusted to 3.0 with hydrochloric acid, and acetone was added to precipitate the echinocandin B nucleus. Centrifuge at 3000 rpm for 15 min with a 120-mesh filter cloth. The crystals of echinocandin B core were collected from the filter cloth, put into a fume hood, and blown with sterile air overnight to obtain a dry solid powder.

[0039] The purity of echinocandin B mother nucleus is 97.9% and the yield is 75% through high-pressure liquid phase detection.

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Abstract

The invention discloses a method for purifying echinocandin B parent nucleus. The method comprises the following steps: 1) performing solid-liquid separation on a conversion solution; 2) concentrating, and removing the moisture from the liquid obtained in the step 1); 3) crystallizing; and 4) separating crystals. The crystallizing method used in the method disclosed by the invention is simple andconvenient to operate, time-saving, low in cost and suitable for continuous production on various scales; the product obtained by crystallization is high in purity; and the adopted non-polar solvent is easily recycled, and the cost is reduced.

Description

technical field [0001] The invention belongs to the field of drug synthesis, and in particular relates to a method for purifying echinocandin B nucleus. Background technique [0002] Fungal infection is a widespread disease that threatens human health, and most of them are superficial infections that occur in mucosal epithelial tissue. Deep fungal infection generally occurs in immunosuppressed people. With the use of organ transplantation and immunosuppressants, open surgery and the abuse of antibiotics, and the spread of human acquired immunodeficiency diseases, the morbidity and fatality rates are increasing. rise. The study of antifungal drugs has also become one of the hot spots in drug research and has gained more and more attention. [0003] Echinocandins are a class of natural antifungal substances, a group of natural products discovered in the 1970s, consisting of a cyclic polypeptide core and fatty acid side chains. Its mechanism of action is to exert its antifun...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K7/56C07K1/36C07K1/34C07K1/30
CPCC07K7/56
Inventor 张贵民薛国希王晓伟
Owner LUNAN PHARMA GROUP CORPORATION
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