High-efficiency separation and purification method for pneumocandin

A technology of separation and purification, nemocontin, applied in the direction of peptides, etc., can solve the problems of difficult environmental control, low process efficiency, low sample load, etc., to solve the problems of insufficient selectivity, good repeatability, and fast separation speed.

Inactive Publication Date: 2018-07-06
浙江华谱新创科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Most of the prior art uses adsorption resin, activated carbon adsorption and ordinary silica gel to remove impurities and purify during the preparation process, which has low proces

Method used

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  • High-efficiency separation and purification method for pneumocandin
  • High-efficiency separation and purification method for pneumocandin
  • High-efficiency separation and purification method for pneumocandin

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0029] Example 1

[0030] 3g of Numocantine crude product, dissolved in 30mL ethanol-water, injection volume 30mL, loading volume 1%; use carboxyl-bonded hydrophilic silica gel column (column specification 50×250mm, particle size 10μm, pore size Packing mass 300g), flow rate 80mL / min; organic solvent is ethanol, in which the volume ratio of organic solvent / water is 90 / 10; UV detector, detection wavelength 210nm, from the peak of the target peak, start to pick up the distillate until the peak returns to the baseline and stop After purification, a product with a purity of Numocantine B0 of over 99.1% and an impurity C0 of less than 0.1% can be obtained.

Example Embodiment

[0031] Example 2

[0032] Other conditions are the same as in Example 1, except that the pore size of the filler is After purification, a product with a purity of Numocantine B0 of 99.8% or more and an impurity C0 of less than 0.1% can be obtained.

Example Embodiment

[0033] Example 3

[0034] Other conditions are the same as in Example 1, except that a carboxyl hydrophilic silica gel column (column size 50×1000mm, particle size 10μm, pore size The packing mass is 1.2kg). After purification, a product with a purity of Numocantine B0 of more than 99.5% and an impurity C0 of less than 0.1% can be obtained.

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Abstract

The objective of the invention is to provide a high-efficiency separation and purification method for pneumocandin. The high-efficiency separation and purification method is characterized in that a hydrophilic silica-gel material surface-modified by polar groups is adopted; a crude pneumocandin product is dissolved by using a mixture of an organic solvent and an aqueous solution in a certain ratio; after sample loading, a mixture of an organic solvent and water in a certain ratio is used for elution; and purification is carried out so as to obtain pneumocandin B0 with chromatographic purity ofmore than 99%, wherein the content of the critical impurity C0 is less than 0.1%. The method provided by the invention realizes high-efficiency separation and purification of pneumocandin B0, has thecharacteristics of good stability, great sample loading amount, simple operation, controllability, etc., and is applicable to industrial separation and purification.

Description

technical field [0001] The invention belongs to the technical field of separation, purification and purification of pneumocidine B0, and in particular provides a high-efficiency separation and purification method of pneumocidine. Background technique [0002] Pneumocandin B0 (pneumocandin B0) is a secondary metabolite produced by Glarealozoyensis. Glarealozoyensis will produce structural analogue A0 and isomer C0 in addition to pneumocandin B0 during fermentation. As the precursor compound of the antifungal drug caspofungin, the preparation of high-purity neumeridine B0 is very important for the purification of caspofungin. [0003] Pneumocidine B0 has a complex structure and is unstable to heat and alkali. It is difficult to remove C0 and A0, which increases the difficulty of preparing high-purity pneumocidine B0. [0004] The structure of Neomercantin is as follows: [0005] [0006] name R1 R2 Neomercontin B0 Oh CH 3 Neomerconti...

Claims

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Application Information

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IPC IPC(8): C07K7/56C07K1/22
CPCC07K7/56
Inventor 周永正吴元华张亮赵芩禾
Owner 浙江华谱新创科技有限公司
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