Method for preparing high-purity 4'-epi-daunorubicin

A technology of epidaunorubicin and concentration, applied in the field of preparing high-purity epidaunorubicin, can solve problems such as complicated steps and the like

Inactive Publication Date: 2011-09-21
SHANGHAI INST OF PHARMA IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The steps of this method are cumbersome, and the reverse chromatography packing with silica gel as the medium must be used to complete the separation and purification process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-2

[0044] Embodiment 1-2 investigates the influence of the fermented liquid of different sources on separation process

Embodiment 1

[0046] The pretreatment process of epidaunorubicin fermented liquid:

[0047] Take 1000ml of fermentation broth, its purity is 1.6%, and the unit is 24ug / ml, adjust the pH of the fermentation broth to 3.0, let it stand for a while, discard the supernatant after high-speed centrifugation, and use 1 times of acetone to soak the surface softness For erythromycin, the mycelium was removed by filtration, and the epidaunorubicin was dissolved in water after evaporating acetone to dryness, and the insoluble matter was removed by filtration similarly, and the purity was detected to be 3.2%.

[0048] The preparation method of epidaunorubicin:

[0049] Install a macroporous weak acid ion-exchange column with a height of about 20 cm and a diameter of about 4 cm, pass the aqueous solution of epidaunorubicin through the column at a flow rate of 2 ml / min, the epidaunorubicin is completely adsorbed on the column, and then use The column was eluted with 1:1 acetone water (0.01M HCl), and the...

Embodiment 2

[0053] The pretreatment process of epidaunorubicin fermented liquid:

[0054] Take 1000ml of fermentation broth, its purity is 2.2%, and the unit is 21ug / ml, adjust the pH of the fermentation broth to 5.0, let it stand for a while, discard the supernatant after high-speed centrifugation, and use 2 times of acetone to soak the surface softness For erythromycin, the mycelium was removed by filtration, and the epidaunorubicin was dissolved in water after evaporating acetone to dryness, and the insoluble matter was removed by filtration similarly, and its purity was detected to be 3.5%.

[0055] The preparation method of epidaunorubicin:

[0056] Install a D152 exchange column with a height of about 20cm and a diameter of about 4cm, pass the aqueous solution of epidaunorubicin through the column at a flow rate of 2ml / min, the epidaunorubicin is completely absorbed on the column, and then use 1:1 The column was eluted with acetone water (0.05M HCl), and all the eluate was collected,...

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Abstract

The invention provides a method for preparing high-purity 4'-epi-daunorubicin, which comprises the following steps of: a) loading the treated 4'-epi-daunorubicin fermentation liquor on macroporous weak acid resin, and eluting by using aqueous solution of acetone or methanol added with hydrochloric acid; b) evaporating the 4'-epi-daunorubicin eluent to dryness, dissolving in water, and extracting by using chloroform; and c) loading the 4'-epi-daunorubicin extracting solution on nonpolar adsorption resin, and eluting by using aqueous solution of acetone to obtain the 4'-epi-daunorubicin. The method has simple steps, is suitable for large-scale industrial production, and has high commercial value; and the final purity of the prepared 4'-epi-daunorubicin is improved to over 97 percent.

Description

technical field [0001] The invention relates to a method for preparing epidaunorubicin, a precursor of antitumor drug epirubicin, in particular to a method for preparing high-purity epidaunorubicin by a microbial fermentation method. Background technique [0002] Daunorubicin and doxorubin and epirubicin synthesized from it are very important anti-tumor anthracycline antibiotics in clinical practice. Epirubicin has lower cardiotoxicity and bone marrow toxicity than doxorubicin, while the antitumor effect is equivalent or higher. Epirubicin (4'-epi-daunorubicin) is an important precursor for industrial production of epirubicin. The difference between it and daunorubicin lies in the configuration of the hydroxyl group at the C4 position of the deoxysugar in the molecule. The chemical synthesis from daunorubicin to epidaunorubicin needs to go through a multi-step reaction process with harsh conditions and will cause environmental pollution. If the microbial fermentation metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/252C07H1/08
Inventor 李继安张志杰卢亮
Owner SHANGHAI INST OF PHARMA IND CO LTD
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