Composite type activated carbon and application thereof in purifying tacrolimus

A technology of tacrolimus and activated carbon, which is applied to composite activated carbon and its preparation and application in purifying tacrolimus, can solve the problems of large amount of elution solvent, low purity and yield, and difficult separation, etc. , to achieve the effect of being conducive to green production, simple operation and simple process

Inactive Publication Date: 2016-08-03
HANGZHOU ZHONGMEI HUADONG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The purpose of the present invention is to overcome the deficiencies in the prior art of purifying and separating tacrolimus fermentation liquid with many impurities, difficult separation, complicated purification methods, long time consumption, low purity and yield, and to

Method used

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  • Composite type activated carbon and application thereof in purifying tacrolimus
  • Composite type activated carbon and application thereof in purifying tacrolimus
  • Composite type activated carbon and application thereof in purifying tacrolimus

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0057] Example 1

[0058] Preparation method of composite activated carbon

[0059] 1) Screening and drying of wood chips

[0060] The crushed wood chips with a moisture content of 40% are sent to a vibrating screen by a bucket elevator to obtain wood chips with a particle size of 6-40 mesh, which are transported to a cyclone separator by a blower, and the separated wood chips fall into a storage bin.

[0061] The sawdust is continuously dropped into the screw feeder quantitatively and continuously from the disc feeder under the storage bin, and the hot air pipe is added to dry the sawdust with hot air at 120~150℃, where the hot air flow rate is 8 m / s; after drying The moisture content of wood chips is 18%.

[0062] 2) Prepare a potassium hydroxide aqueous solution with a concentration of 70%.

[0063] 3) Kneading

[0064] The sawdust after drying in step 1) is kneaded with the potassium hydroxide aqueous solution in step 2) under stirring; the weight ratio of the sawdust to the potassiu...

Example Embodiment

[0071] Example 2

[0072] Take 1000g of fermentation broth and extract with 7L ethanol to obtain about 60g of concentrated solution, dilute with ethyl acetate to 500ml, add 500ml of 2% NaOH aqueous solution, and keep at 50°C for 3 hours and separate into ethyl acetate phase; Add 500 ml of 1% NaOH aqueous solution to the ethyl ester phase, stir evenly and let stand overnight.

[0073] The next day, the extract was separated, and 12 g of the composite activated carbon prepared according to Example 1 was added, stirred at room temperature for 1 hour, filtered, and rinsed with an appropriate amount of ethyl acetate to obtain 700 ml of the filtrate.

[0074] Concentrate the filtrate to about 40g, add 30ml ethyl acetate to dissolve it, keep stirring for 1h, add 40ml purified water and 160ml n-hexane in batches within 1h, continue stirring for 1h, and let stand overnight.

[0075] Filter the crystalline liquid, wash with 40ml n-hexane and 40ml pure water respectively, and dry at 50~70℃ to ob...

Example Embodiment

[0076] Example 3

[0077] 1) Take 2500g of fermentation broth and extract with 20L of acetone to obtain about 150g of concentrated solution, dilute to 1800ml with ethyl formate, and add 600ml of 1% Na 2 CO 3 The aqueous solution was kept at 50°C for 3 hours and then separated.

[0078] 2) After layering, add 600ml 0.5% Na to the ethyl formate phase 2 CO 3 , Stir well and let stand overnight.

[0079] 3) The next day, the extract was separated, 40 g of the composite activated carbon prepared according to this Example 1 was added, stirred at room temperature for 1 hour, filtered, and rinsed with a proper amount of ethyl formate to obtain the filtrate.

[0080] 4) Concentrate the filtrate to about 100g, add 100ml of acetone to dissolve, stir at room temperature for 1h, add 50ml of purified water and 500ml of n-heptane in batches within 0.5h, continue to stir for 1h, and let it stand overnight.

[0081] 5) Filter the crystalline liquid, wash with 100ml n-heptane and 100ml pure water, and dr...

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Abstract

The invention relates to the technical field of drug preparation and discloses composite type activated carbon and the application thereof in purifying tacrolimus. Through fermentation broth filtration, drying, digestion, extraction and washing, composite type activated carbon decoloration and decontamination, and crystal purification, the problems of existing tacrolimus purifying methods that purification yield is low, time consumption is high, elution solvent consumption is high, pollution is serious, and industrialized production can not be achieved easily are solved. By the adoption of the composite type activated carbon and the application thereof in purifying tacrolimus, large-scale production can be achieved easily, solvent consumption is low, production cycle is short, an obtained tacrolimus crude product is high in purity and is white or off-white color powder, weight fraction is 85% or more, and HPLC normalized concentration is 90% or more.

Description

technical field [0001] The invention relates to the technical field of medicine preparation, in particular to a composite activated carbon and its preparation and application in purifying tacrolimus. Background technique [0002] Tacrolimus is a new type of potent macrolide immunosuppressant. In 1991, Japan developed Tacrolimus capsules and injections called Prograf, which were officially launched for primary Treatment of rejection in liver and kidney transplants, and later approved for bone marrow transplantation. At present, tacrolimus preparations have been marketed in more than 80 countries including China, Japan, and the United States, and are widely used in anti-rejection therapy after solid organ transplantation such as liver, pancreas, kidney, heart, and lung. In 1999, tacrolimus ointment was put on the Japanese market for the treatment of atopic dermatitis in adults. [0003] Tacrolimus is a fermentation product isolated from Streptomyces spp. (streptomycestsukuba...

Claims

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Application Information

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IPC IPC(8): C01B31/12C07D498/18
CPCC01B32/30C01B32/312C07D498/18
Inventor 高庆峰吴萍诸敏吴文艺龚胜张旭军
Owner HANGZHOU ZHONGMEI HUADONG PHARMA
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