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Method for separating and purifying fidaxomicin

A non-damicin, separation and purification technology, applied in the field of separation and purification, can solve the problems of poor separation effect, low purification efficiency, complicated operation, etc., and achieve the effects of improved purity and recovery rate, simple operation and good separation effect.

Active Publication Date: 2015-04-15
JIANGSU SENRAN CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires two silica gel column chromatography and ODS reversed-phase medium pressure liquid chromatography, which is cumbersome and expensive
[0007] The disadvantages of low purification efficiency, low recovery rate, poor separation effect and cumbersome operation generally exist in the prior art

Method used

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  • Method for separating and purifying fidaxomicin
  • Method for separating and purifying fidaxomicin
  • Method for separating and purifying fidaxomicin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Sample solution preparation

[0024] Get 65g non-damicin crude product (HPLC spectrogram is attached figure 1 shown), dissolved in 650ml glacial acetic acid, filtered with 0.45μm polytetrafluoroethylene ethylene filter membrane after dissolving, and the filtrate was further mixed with 650ml acetonitrile-1% glacial acetic acid aqueous solution (the volume ratio of acetonitrile to 1% glacial acetic acid aqueous solution is 45:55) was diluted to 50 mg / ml as a next step to prepare a sample solution of non-damicin.

[0025] (2) Separation and purification:

[0026] Inject 1300ml of the solution diluted in step (1) into a reversed-phase HPLC preparative chromatograph (using a glass column with an inner diameter of 200cm and a height of 25cm, and UniSil 10-120-C8 reversed-phase silica gel as a chromatographic filler, the dosage is 4kg, first Rinse 2 column volumes (CV) with 45% acetonitrile in water, then equilibrate with 20% acetonitrile for 2 CV), the mobile phase con...

Embodiment 2

[0030] According to the method of step (1) in Example 1, prepare the sample solution of non-damicin, and inject 13000ml of the diluted solution into the reversed-phase high-performance liquid phase preparative chromatograph (using a glass column with an inner diameter of 200cm and a height of 25cm, UniSil 10-120-C8 reversed-phase silica gel is used as a chromatography filler, the dosage is 4kg, first wash 2 column volumes CV with 45% acetonitrile aqueous solution, and then equilibrate 2 CVs with 20% acetonitrile), the mobile phase consists of acetonitrile-water ( Containing 1% glacial acetic acid), gradient elution is carried out on the stationary phase, that is, during 0~50min, the volume ratio of acetonitrile-1% glacial acetic acid aqueous solution is 40:60; during 51~150min, the volume ratio of acetonitrile-1% ice The volume ratio of the acetic acid aqueous solution is 50:50; the flow rate is 800ml / min, the ultraviolet detector is detected online, and the detection wavelengt...

Embodiment 3

[0033] (1) Preparation of sample solution:

[0034] Get 65g non-damicin crude product (HPLC spectrogram is attached figure 1shown), dissolved in 650ml of glacial acetic acid, filtered with a 0.45μm polytetrafluoroethylene ethylene filter membrane after dissolution, and the filtrate was further mixed with 650ml of acetonitrile-1% glacial acetic acid aqueous solution (the volume ratio of acetonitrile-1% glacial acetic acid aqueous solution is 45 :55) was diluted to 50 mg / ml as a next step to prepare a sample solution of non-damicin.

[0035] (2) Separation and purification of samples

[0036] Inject 1300ml of the solution diluted in step (1) into a reversed-phase HPLC preparative chromatograph (using a glass column with an inner diameter of 200cm and a height of 25cm, and SP-100-8-C8-HP reversed-phase silica gel as a chromatographic filler, with an amount of 4kg, wash 2 column volume CVs with 45% acetonitrile aqueous solution, and then equilibrate 2 CVs with 20% acetonitrile)...

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Abstract

The invention provides a method for separating and purifying fidaxomicin. The method comprises the following steps: taking the C8 reverse phase silica gel as the filling material, carrying out column chromatography, dissolving fidaxomicin by acetic acid, loading the solution into the column, eluting the solution by a mobile phase, and collecting the sample; after the separation and purification, the HPLC purity of fidaxomicin is not less than 99.5%, and the content of a single impurity is not larger than 0.10%. The provided purification method of fidaxomicin adopts a novel medium having high selectivity and high capacity, thus the column has a high efficiency, the resolution is high, the separation and purification effect is better, the retention time is shorter, the elution agent using amount is less, and moreover the shortages that the fidaxomicin purity is low and the fidaxomicin quality is bad due to the low column efficiency and bad separation degree are overcome.

Description

technical field [0001] The invention relates to a method for separation and purification, in particular to a method for separation and purification of high-purity non-damicin, in particular to a method for separation and purification of non-damicin with an HPLC purity of more than 99%. Background technique [0002] Fidamicin (common name: fidaxomicin, trade name: Dificid) is an 18-membered macrolide antibiotic produced by Cystium citridioides ( Dactylosporangium aurantiacum ) obtained by fermentation, belonging to Tiacumicins (Tiacumicins) compounds. Fidamicin was developed by Optimer and was approved by the FDA on May 27, 2011. It is the first FDA-approved treatment of Clostridium difficile (Clostridium difficile)-associated diarrhea (CDAD) in more than 20 years of antibiotics. Its mechanism of action is novel, mainly through the inhibition of bacterial RNA polymerase to produce a rapid anti-refractory Clostridium infection (CDI) effect. Its treatment of CDI is superior ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08C07H1/06
Inventor 袁建栋黄仰青姚翠萍
Owner JIANGSU SENRAN CHEM
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