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Method for preparing pneumocandins B0 by adopting dynamic axial compression column system

An axial compression and dynamic technology, applied in the preparation method of peptides, chemical instruments and methods, peptides, etc., can solve the problems affecting the quality of carpafungin, unfavorable production application, and affecting production costs, etc., to achieve easy control, column The effect of bed stability and long service life

Inactive Publication Date: 2015-04-29
JIANGSU HANBON SCI & TECH CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Chinese invention patents 200910133118.0 and 201110266790.4 both disclose the preparation of pneumocidine B by purification with resin column technology 0 method, but none of the related substances (such as: C 0 ) detection and purity control are described, the C in the general fermentation broth 0 The impurity content is about 10%, if not effectively controlled, the obtained B 0 and C 0 The mixture will seriously affect the quality of carpafungin in the next step of synthesis reaction
[0004] Although the method disclosed in Chinese invention patent 201410051009.5 is for C 0 Impurities have been tested and their purity controlled, but their recovery rate is not high, only about 30-40%, and TLC is used to monitor, the operation is complicated, and the effluent needs to be divided into small portions (such as 100ml for each small cup received) for HPLC detection, not conducive to actual production application
And it adopts the traditional chromatographic column, the elution time is long, the column efficiency is low, and the service life is short, which will affect the production cost

Method used

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  • Method for preparing pneumocandins B0 by adopting dynamic axial compression column system
  • Method for preparing pneumocandins B0 by adopting dynamic axial compression column system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] 1. Adjust the pH of the fermented liquid containing neomocontin to 2 for acid precipitation treatment, leach after filtration, centrifuge, add activated carbon for decolorization to obtain a colorless filtrate;

[0015] 2. Homogenize 20 μm silica gel with isopropanol, put it into a dynamic axial compression column, the column packing pressure is 6Mpa, and the column packing size is Φ50×250mm;

[0016] 3. Concentrate and dry the colorless filtrate obtained in step 1, add chloroform / methanol mixture (volume ratio 1:5) to dissolve and obtain a sample liquid, pump it into a dynamic axial compression column to prepare a chromatographic system, and use chloroform / methanol / water mixed solution for elution, the volume ratio of the eluent is 78 / 18 / 1, and the sample loading is 0.2 times the weight of the loaded silica gel. During the elution process, an ultraviolet detector was used for on-line monitoring with a wavelength of 280nm. According to the chromatogram, fractions with ...

Embodiment 2

[0018] 1. Adjust the pH of the fermented liquid containing neomocontin to 3 for acid precipitation treatment, leach after filtration, centrifuge, add activated carbon to decolorize to obtain a colorless filtrate;

[0019] 2. Homogenize 50 μm silica gel with isopropanol, put it into a dynamic axial compression column, the column packing pressure is 8Mpa, and the column packing size is Φ150×250mm;

[0020] 3. Concentrate and dry the colorless filtrate obtained in step 1, add chloroform / methanol mixture (volume ratio 1:4) to dissolve and obtain a sample liquid, pump it into a dynamic axial compression column to prepare a chromatographic system, and use chloroform / methanol / water mixture for elution, the volume ratio of the eluent is 82 / 17 / 3, and the sample loading is 0.25 times of the weight of the loaded silica gel. During the elution process, an ultraviolet detector was used for on-line monitoring with a wavelength of 300nm. According to the chromatogram, fractions with an elut...

Embodiment 3

[0022] 1. Adjust the pH of the fermented liquid containing neomocontin to 4 for acid precipitation treatment, leach after filtration, centrifuge, add activated carbon for decolorization to obtain a colorless filtrate;

[0023] 2. Homogenize the 75μm silica gel with isopropanol, put it into a dynamic axial compression column, the column packing pressure is 10Mpa, and the column packing size is Φ300×250mm;

[0024] 3. Concentrate and dry the colorless filtrate obtained in step 1, add chloroform / methanol mixture (1:4.5 by volume) to dissolve the sample liquid, pump it into a dynamic axial compression column to prepare a chromatographic system, and use chloroform / methanol / water mixed solution for elution, the volume ratio of the eluent is 81 / 18 / 2, and the sample loading is 0.3 times the weight of the loaded silica gel. During the elution process, an ultraviolet detector was used for on-line monitoring with a wavelength of 290nm. According to the chromatogram, fractions with an el...

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Abstract

The invention provides a preparation method of pneumocandins B0. The method comprises the following steps: (1) performing acid precipitation, centrifugation and decoloring pretreatment on a fermentation broth containing pneumocandins B0 to obtain a pneumocandins crude product; (2) packing by adopting a dynamic axial compression column; and (3) pumping the pneumocandins crude product into the dynamic axial compression column, performing online monitoring by using an ultraviolet detector, collecting an objective elution component, and concentrating and drying to obtain pneumocandins B0. The dynamic axial compression column adopted by the method provided by the invention is convenient to operate and can be used for realizing online monitoring, the amount of an elution solvent can be greatly reduced, the elution time is shortened, and the service life of a chromatographic column is ensured at the same time, so that the production cost is reduced, C0 can be effectively removed at the same time, the product recovery rate is high, and the purity can be up to 99% or higher.

Description

technical field [0001] The present invention relates to a kind of preparation carpafungin precursor-neumocondine B 0 The purification method belongs to the field of medicinal chemistry. Background technique [0002] Neomercontin B 0 is made of mold Glarea lozoyensis Secondary metabolites from fermentation. In addition to B0, the fermentation broth also contains C 0 Equal components, pneumocontin B 0 It is mainly used in the synthesis of the drug carpafungin. [0003] Chinese invention patents 200910133118.0 and 201110266790.4 both disclose the preparation of pneumocidine B by purification with resin column technology 0 method, but none of the related substances (such as: C 0 ) detection and purity control are described, the C in the general fermentation broth 0 The impurity content is about 10%, if not effectively controlled, the obtained B 0 and C 0 The mixture will seriously affect the quality of carpafungin in the next step of synthetic reaction. [0004] Altho...

Claims

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Application Information

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IPC IPC(8): C07K7/56C07K1/14
Inventor 张宇关正娟刘大伟张大兵李胜迎金新亮
Owner JIANGSU HANBON SCI & TECH CO
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