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Method for one-step refining of tacrolimus, dihydrotacrolimus and ascomycin in crude tacrolimus

A technology of dihydrotacrolimus and tacrolimus, which is applied in the field of bioengineering, can solve the problem that the small product ascomycin and pure dihydrotacrolimus cannot be obtained, the research is still blank, and the product yield is low and other problems, to achieve the effect of convenient operation, simple process and low cost

Inactive Publication Date: 2018-07-06
TIANJIN LINGSHI BIOTECH DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no report on the one-step purification of tacrolimus active ingredients tacrolimus, dihydrotacrolimus, and ascomycin in the separation and extraction of tacrolimus abroad, and the process of separation and purification of tacrolimus Often complicated, two or more chromatographic purifications are used, the solvent consumption is high, and the product yield is low. The key is that the small product ascomycin and the pure product of dihydrotacrolimus cannot be obtained.
One-step purification of high-efficiency tacrolimus active ingredients tacrolimus, dihydrotacrolimus, and ascomycin has not been reported at home and abroad, and the research on this technology is still blank

Method used

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  • Method for one-step refining of tacrolimus, dihydrotacrolimus and ascomycin in crude tacrolimus
  • Method for one-step refining of tacrolimus, dihydrotacrolimus and ascomycin in crude tacrolimus
  • Method for one-step refining of tacrolimus, dihydrotacrolimus and ascomycin in crude tacrolimus

Examples

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Effect test

example 2

[0029] 1) Fill a 150-mesh self-made polystyrene-divinylphenyl polymer network structure microsphere chromatography filler in a stainless steel chromatography column, configure an eluent solution: acetone:water 60:40, and add a development layer for medicine After adding 5% KH2PO4, adjust the pH to 4.5 with phosphoric acid. The total amount of configuration is 5 times the volume of the stainless steel chromatography column. Equilibrate the column with one volume of the column bed volume of eluent.

[0030] 2) Fully dissolve tacrolimus coarse powder with 80% content in 80% acetone solution at 50 degrees until the concentration of tacrolimus is 250,000 units / mL, add medicinal spreading agent 5% KH2PO4 to dissolve and filter Column material.

[0031] 3) Control the flow rate of the lower column of the chromatography column, slowly and evenly add the dissolved and filtered coarse powder solution from the head of the chromatography column, and then pass through the column chromato...

example 3

[0036]1) Fill a 150-mesh self-made polystyrene-divinylphenyl polymer network structure microsphere chromatography filler in a stainless steel chromatography column, and configure an eluent solution: 1) Acetone: water 57:43, for adding medicine The developing agent is 5% KH2PO4, and then the pH is adjusted to 4.5 with phosphoric acid, and the volume is 3 column bed volumes. 2) Prepare the eluent solution: acetone: water 62:38, add 5% KH2PO4 as a spreading agent for medicine, adjust the pH to 4.5 with phosphoric acid to make the volume of 2 column beds 3) prepare the eluent solution: acetone: water 70 : 30, after adding 5% KH2PO4 as a spreading agent for medicine, adjust pH=4.5 with phosphoric acid, and the volume is 1.5 column bed volumes. First, use acetone:water 57:43 to perform column equilibration with an eluent equal to the volume of the chromatography column bed.

[0037] 2) Fully dissolve tacrolimus coarse powder with 80% content in 80% acetone solution at 50 degrees un...

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Abstract

The invention relates to a method for one-step refining of tacrolimus, dihydrotacrolimus and ascomycin in crude tacrolimus. The method comprises the following steps: developing the crude tacrolimus inthe head of a stainless steel chromatographic column filled with a special packing material, performing chromatographic elution with an eluent containing a solvent and water according to a ratio of 60:40, having a pH value, adjusted with an acid, of 4.5 and also containing 5% of a developer, and performing distribution collection, pure product concentration, crystallization and recrystallizationto obtain pure tacrolimus, pure dihydrotacrolimus and pure ascomycin. The HPLC purity of the tacrolimus, dihydrotacrolimus and ascomycin which are obtained through the method is more than 98%. The method has the advantages of convenience in operation, simple process and low cost, can be used in pilot production, and is very suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of bioengineering, and specifically relates to a method for separating and purifying fermentation products, in particular to a method for one-step refining of tacrolimus, dihydrotacrolimus and ascomycin, the medicinal components in crude tacrolimus. Background technique [0002] Tacrolimus (tacrolimus, FK506) is a new type of twenty-eight bacterium extracted from the fermentation broth of Streptomyces tsukubaensis No.9993 isolated from the soil of Mt. Three-membered macrolide polyketide immunosuppressant. Clinical studies have shown that its immunosuppressive activity is 10-100 times that of the traditional immune agent cyclosporine A. At present, it has been widely used in liver, bone marrow transplantation, prevention and treatment of rejection of other drug-resistant kidney transplantation, Behcet's disease, degenerative dermatitis, psoriasis, ichthyosis, alopecia areata, rheumatoid arthritis, psoriasis, multiple ...

Claims

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Application Information

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IPC IPC(8): C07D498/18
CPCC07D498/18
Inventor 闻建华闻铭远傅红
Owner TIANJIN LINGSHI BIOTECH DEV CO LTD
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