Purifying method for high-purity echinocandin B mother nucleus or salt thereof

An echinocandin, high-purity technology, applied in the field of medicine, can solve the problems of easily polluting the environment, increasing production costs, etc., achieving good separation effect, preventing decomposition and damage, and overcoming easy decomposition or incomplete elution effect.

Inactive Publication Date: 2018-03-06
JIANGSU SENRAN CHEM +1
View PDF4 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method is suitable for large-scale production, a large amount of solvent is used in the ex

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Purifying method for high-purity echinocandin B mother nucleus or salt thereof
  • Purifying method for high-purity echinocandin B mother nucleus or salt thereof

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0036] Example 1 Method for preparing high-purity echinocandin B from crude echinocandin B mother nucleus (content 85%)

[0037] Measure 9g of the crude echinocandin B mother nucleus and dissolve it in 90ml of purified water, and ultrasonically assist it. After the solution is clarified, filter it with a 0.45um water-based filter membrane, and collect the filtrate and store it at 2-15°C for later use. A 50mm*250mm dynamic axial compression preparative column (50DAC for short) is used, and Daisogel SP-100-8-ODS-P is used as the preparative column packing. Before loading the sample, pre-column the pre-column pre-column, first rinse with 100% methanol solution for 1.5 column volumes to remove impurities, and then equilibrate the pre-column with 1.5 column volumes with methanol:0.5% acetic acid aqueous solution=3:97. Then use methanol: 1% acetic acid aqueous solution=5:95 to flush 3 column volumes, and then use methanol: 1.5% acetic acid aqueous solution=8:92 to flush 4 column volum...

Example Embodiment

[0038] Example 2 Method for preparing high-purity echinocandin B from crude echinocandin B mother nucleus (content 90%)

[0039] Measure 9g of the crude echinocandin B mother nucleus and dissolve it in 90ml of purified water, and ultrasonically assist the solution. After the solution is clarified, filter it with a 0.45um water-based filter membrane, and collect the filtrate and store it at 2-15°C for later use. A 50mm*250mm dynamic axial compression preparative column (50DAC for short) is used, and Daisogel SP-100-8-ODS-P is used as the preparative column packing. Before loading the sample, pre-column the pre-column pre-column, rinse with 100% methanol solution for 1.5 column volumes to remove impurities, and then equilibrate the pre-column with methanol: 0.5% TFA aqueous solution = 3:97 for 1.5 column volumes. Then use methanol: 1% TFA aqueous solution=4:96 to flush 2.5 column volumes, and then use methanol: 1.5% TFA aqueous solution=6:94 to flush 3.5 column volumes. When the p...

Example Embodiment

[0040] Example 3 Method for preparing high-purity echinocandin B from crude echinocandin B mother nucleus (content 95%)

[0041] Measure 9g of the crude echinocandin B mother nucleus and dissolve it in 90ml of purified water, and ultrasonically assist it. After the solution is clarified, filter it with a 0.45um water-based filter membrane, and collect the filtrate and store it at 2-15°C for later use. A 50mm*250mm dynamic axial compression preparative column (50DAC for short) is used, and Daisogel SP-100-8-ODS-P is used as the preparative column packing. Before loading the sample, perform pre-column pretreatment on the preparative column, first rinse with 100% methanol solution for 1.5 column volumes to remove impurities, and then equilibrate the preparative column with 1.5 column volumes of methanol: 0.3% phosphoric acid aqueous solution = 2:98. Then use methanol: 0.8% phosphoric acid aqueous solution=4:96 to flush 4 column volumes, and then use methanol: 1.2% phosphoric acid a...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention provides a purifying method for a high-purity echinocandin B mother nucleus or a salt thereof. The purifying method comprises the following steps: dissolving a crude product of an echinocandin B mother nucleus or a salt thereof to prepare a sample and loading the sample into a preparative high-performance liquid chromatographic column; carrying out elution with mixed liquor of an aqueous solution and an organic solvent as a mobile phase; and fractionally collecting eluates. The purifying method is simple to operate, high in purifying efficiency and easy in process flow; the recovery rate of the high-purity echinocandin B mother nucleus or the salt thereof is more than 85%; a small amount of organic solvents are used, so the method is friendly to environment; the method has good process reproducibility, can realize mass product, is high and stable in recovery rate and saves cost; product purity reaches 99% or above; the process of separation and purification is simple; andthe concentration of an organic phase is low, so elution time is short, and cost is saved.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a method for purifying a high-purity echinocandin B nucleus or a salt thereof. Background technique [0002] The morbidity and mortality of fungal infection diseases, especially deep fungal infection diseases, are increasing year by year, so the research and development of antifungal drugs will become a difficult problem for human beings. Echinocandins are a group of natural products discovered in the 1970s, composed of similar cyclic polypeptide cores and different fatty acid side chains, inhibit B.(1,3)-D in the cell wall through non-competitive effects -Synthesis of glucose sugar, thus exerting antifungal action. Echinocandins have a unique mechanism of action, low adverse reaction rate, and strong antibacterial activity against some azole and amphotericin B-resistant fungi. [0003] Under the action of deacylase, echinocandin B cuts off the acyl side chain to generate echi...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07K7/56C07K1/16
CPCC07K7/56
Inventor 袁建栋黄仰青顾家宁孙占莉
Owner JIANGSU SENRAN CHEM
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap