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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
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method is suitable for large-scale production, a large amount of solvent is used in the extraction process, which not only increases the production cost, but also easily pollutes the environment.

Method used

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  • 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

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Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1 is the method for preparing high-purity echinocandin B by echinocandin B mother nucleus crude product (content 85%)

[0037] Take 9g of the crude echinocandin B nucleus and dissolve it in 90ml of purified water, and dissolve it with ultrasonic waves. After the solution is clarified, filter it with a 0.45um water-based filter membrane, collect the filtrate and store it in an environment of 2-15°C until use. A 50mm*250mm dynamic axial compression preparative column (50DAC for short) was used, and Daisogel SP-100-8-ODS-P was used as the preparative column packing. Before loading the sample, perform pre-column pretreatment on the preparative column, wash 1.5 column volumes with 100% methanol solution to remove impurities, and then equilibrate 1.5 column volumes of the preparative column with methanol:0.5% acetic acid aqueous solution=3:97. Then use methanol:1% acetic acid aqueous solution=5:95 to wash 3 column volumes, then use methanol:1.5% acetic acid aqueou...

Embodiment 2

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

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

Embodiment 3

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

[0041] Take 9g of the crude echinocandin B nucleus and dissolve it in 90ml of purified water, and dissolve it with ultrasonic waves. After the solution is clarified, filter it with a 0.45um water-based filter membrane, collect the filtrate and store it in an environment of 2-15°C until use. A 50mm*250mm dynamic axial compression preparative column (50DAC for short) was used, and Daisogel SP-100-8-ODS-P was used as the preparative column packing. Before loading the sample, pre-column pretreatment was performed on the preparative column. First, 1.5 column volumes were washed with 100% methanol solution to remove impurities, and then 1.5 column volumes of the preparative column were equilibrated with methanol:0.3% phosphoric acid aqueous solution=2:98. Then use methanol: 0.8% phosphoric acid aqueous solution=4:96 to wash 4 column volumes, then use met...

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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

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Application Information

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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
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