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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 provide a composite activated carbon Its application in the purification of tacrolimus solves the problems of low purification yield, long time consumption, large amount of elution solvent, high pollution and unfavorable industrialized production in the existing purification method

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

Embodiment 1

[0058] Preparation method of composite activated carbon

[0059] 1) Screening and drying of sawdust

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

[0061] The wood chips are quantitatively and continuously dropped into the screw feeder from the disc feeder under the silo, and then fed into the hot air pipe, and the wood chips are air-dried in hot air at 120-150 °C, and the hot air flow rate is 8 m / s; after drying The wood chips have a moisture content of 18%.

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

[0063] 3) Kneading

[0064] Kneading the dried sawdust in step 1) with the aqueous potassium hydroxide solution in step 2) under stirring; the weight ratio of the sawdust to the aque...

Embodiment 2

[0072] Take 1000g of fermentation broth bacteria residue, extract with 7L of ethanol to obtain about 60g of concentrated solution, dilute to 500ml with ethyl acetate, add 500ml of 2% NaOH aqueous solution, keep at 50°C for 3 hours and then separate to obtain the ethyl acetate phase; Add 500 ml of 1% NaOH aqueous solution to the ethyl ester phase, stir well 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, rinsed with an appropriate amount of ethyl acetate, and 700 ml of filtrate was obtained.

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

[0075] Filter the crystallization solution, wash with 40ml of n-hexane and 40ml of pure water respe...

Embodiment 3

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

[0078] 2) After layering, add 600ml of 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, and 40 g of the composite activated carbon prepared in Example 1 was added, stirred at room temperature for 1 h, filtered, and rinsed with an appropriate amount of ethyl formate to obtain the filtrate.

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

[0081] 5) Filter the crystallization solution, wash with 100ml of n-heptane and 100ml of pure water respectivel...

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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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