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Purification method for pneumocandin B0 with few solid wastes

A purification method and waste technology, which are applied in the preparation methods of peptides, chemical instruments and methods, and organic chemistry, etc., can solve the problems of many solid wastes, affect the environment, and low purity, and achieve the effect of reducing the amount of production.

Pending Publication Date: 2021-05-04
SUZHOU NO 4 PHARMA FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The biggest shortcoming is that the amorphous silica gel used in chromatography can only be used once, resulting in a lot of solid waste generated in the production process, which affects the environment; and its purity is still low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) plate-and-frame filter the fermented liquid of Neomocontin B0, collect the mycelia, extract the mycelia with methanol, and filter to obtain the extract;

[0023] (2) Adsorb the extract with XR910 resin, rinse with 5 times the column bed volume of methanol with a volume ratio of 60% after the adsorption is completed, and then use 3 times the column bed volume for methanol elution, and the eluent is heated at 45 ° C. Concentrate under reduced pressure in a vacuum environment to obtain a concentrate;

[0024] (3) The concentrate is chromatographed on spherical silica gel, and a 4:1 dichloromethane-methanol mixture is used as a mobile phase development layer to obtain a chromatographic solution;

[0025] (4) The chromatographic solution was distilled under reduced pressure at 45° C. to obtain the finished product of Neomocontin B0 (purity: 99.2 wt%).

Embodiment 2

[0027] (1) plate-and-frame filter the fermented liquid of Neomocontin B0, collect the mycelia, extract the mycelia with methanol, and filter to obtain the extract;

[0028] (2) Adsorb the extract with XR910 resin, rinse with 6 times of the column bed volume volume ratio of 60% methanol after the adsorption, then elute with 4 times of the column bed volume of methanol, and store the eluent at 45°C Concentrate under reduced pressure in a vacuum environment to obtain a concentrate;

[0029] (3) The concentrate is chromatographed on spherical silica gel, and a 4:1 dichloromethane-methanol mixture is used as a mobile phase development layer to obtain a chromatographic solution;

[0030] (4) The chromatographic solution was distilled under reduced pressure at 45° C. to obtain the finished product of Neomocontin B0 (purity: 99.3 wt%).

Embodiment 3

[0032] (1) plate-and-frame filter the fermented liquid of Neomocontin B0, collect the mycelia, extract the mycelia with methanol, and filter to obtain the extract;

[0033] (2) Adsorb the extract with XR910 resin, rinse with methanol with a volume ratio of 7 times the column bed volume of 60% after the adsorption is completed, and then elute with methanol of 5 times the column bed volume, and the eluent is heated at 45 ° C. Concentrate under reduced pressure in a vacuum environment to obtain a concentrate;

[0034] (3) The concentrate is chromatographed on spherical silica gel, and a 4:1 dichloromethane-methanol mixture is used as a mobile phase development layer to obtain a chromatographic solution;

[0035] (4) The chromatographic solution was distilled under reduced pressure at 45° C. to obtain the finished product of Neomocontin B0 (purity: 99.5 wt%).

[0036] It can be seen from Examples 1-3 that this purification method can make the purity of the finished product of Neo...

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Abstract

The invention belongs to the technical field of organic matter purification, and relates to a purification method for pneumocandin B0 with few solid wastes. The method comprises the following steps of extraction, resin adsorption separation, spherical silica gel chromatography and vacuum concentration. The purity of the finished pneumocandin B0 prepared by the method can be increased to 99wt% or above, and spherical silica gel can be repeatedly used, so that the output of solid wastes in production can be greatly reduced, and the method is more environment-friendly.

Description

technical field [0001] The invention relates to the technical field of organic matter purification, in particular to a method for purifying pneumocidine B0 with less solid waste. Background technique [0002] Neomocontin B0 is an intermediate of caspofungin acetate, which is one of the important raw materials in current biopharmaceutical products. Its production and preparation are mainly obtained through fungal fermentation, synthesis and purification. In the current production process of pneumocidine B0, there are great differences in the fungal fermentation raw materials and processes used, as well as the raw materials and processes used in the later purification operations. Therefore, the quality stability and reliability of the current pneumocidine B0 product are relatively poor, and several are reflected in the poor purity stability of the pneumocidine B0 product, which seriously affects the use quality of the pneumocidine B0 product. [0003] The preparation method o...

Claims

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Application Information

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IPC IPC(8): C07K7/56C07K1/36C07K1/34C07K1/16
CPCC07K7/56
Inventor 刘永胜胡宁刘小艳李艳琴
Owner SUZHOU NO 4 PHARMA FACTORY
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