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Method for obtaining high purity echinocandin D

A high-purity echinocandin technology, applied in the field of obtaining high-purity echinocandin D, can solve the problems of high cost, difficulty in large-scale application, and low yield

Inactive Publication Date: 2012-05-23
SHANGHAI INST OF PHARMA IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The echinocandin D obtained by this method contains impurities such as pigments (the color is yellow or light yellow), the purity is about 70%-90%, the yield is low (40-60%), and a large amount of acetonitrile, Chloroform is a toxic reagent with high cost and is difficult to apply on a large scale

Method used

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  • Method for obtaining high purity echinocandin D
  • Method for obtaining high purity echinocandin D

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] Load 100g NM-PS100 (4×20cm) reversed-phase column, dissolve 0.5g sample containing 80% echinocandin D in 60% methanol aqueous solution, pass through the column, echinocandin D is completely adsorbed on the column, The column was eluted with 85% methanol aqueous solution, and the higher purity fractions in the eluate were collected by distribution. The HPLC purity was 95.5%, the yield was 98%, and it was white. See attached figure 1 .

Embodiment 2

[0070] Example 2 (Influence of methanol concentration used for sample loading on purification)

[0071] Load 100g of NM-PS100 (4×20cm) reversed-phase column, dissolve 0.5g of sample containing 80% echinocandin D in 70% methanol aqueous solution, pass through the column, echinocandin D is completely adsorbed on the column, The column was eluted with 85% methanol aqueous solution, and the higher-purity fraction in the eluate was distributed and collected. The detected purity was 92%, the yield was 98%, and it was pale yellow.

Embodiment 3

[0072] Example 3 (Influence of methanol concentration used for sample loading on purification)

[0073] Load 100g NM-PS100 (4×20cm) reversed-phase column, dissolve 0.5g sample containing 80% echinocandin D in 50% methanol aqueous solution, pass through the column, echinocandin D is completely adsorbed on the column, The column was eluted with 85% methanol aqueous solution, and the higher purity fractions in the eluate were distributed and collected. The detected purity was 95%, the yield was 98%, and it was white.

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Abstract

The invention discloses a method for obtaining high purity echinocandin D. The method comprises the steps of: (1) mixing a solution containing an echinocandin D crude product with a methanol aqueous solution 1 so as to obtain a solution 1; (2) loading the solution 1 to a reversed-phase chromatography column; and (3) conducting elution with a methanol aqueous solution 2, thus obtaining the high purity echinocandin D.

Description

technical field [0001] The present invention relates to a purification method of a compound, in particular to a method for obtaining high-purity echinocandin D. Background technique [0002] Echinocandins are a class of natural cyclic lipopeptide compounds with a cyclic hexapeptide core and fatty acid side chain structure discovered in the 1970s. According to the different substituents and fatty acid side chains on the cyclic hexapeptide, it is divided into different compounds. Echinocandins belong to a new class of antifungal compounds. As glucan synthase inhibitors, they play a bactericidal effect by non-competitively inhibiting the synthesis of β-(1,3)-D-glucan in fungal cell walls. . Many similar components are produced during fermentation (US Pat. No. 4,024,245). Among them, echinocandin D has a similar bacteriostatic activity to echinocandin B, so it has development value (US Pat. Nos. 4,024,245, 495,878, 495,652). However, the yield of echinocandin D is higher than...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K7/56C07K1/20
Inventor 胡海峰闵涛玲朱宝泉
Owner SHANGHAI INST OF PHARMA IND
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