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Method for separating and purifying fidaxomicin

A technology for separation and purification of fidaxomicin, applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., can solve the problems of large solvent consumption, high production cost, and reduced resin exchange capacity, and achieve simple and easy process Easy to use, low production cost, environmentally friendly effect

Active Publication Date: 2019-01-22
CHENGDU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the extract enters the next macroporous adsorption resin, these oils will be adsorbed on the resin, which greatly reduces the resin exchange capacity; the elution of fidaxomicin is seriously tailed, and the effective separation of fidaxomicin and impurities cannot be achieved. Additional steps to remove impurities; solvent-intensive to remove grease when regenerating resin
The above patents all use preparative column chromatography to further separate the impurities of fidaxomicin, which has high production costs and is not conducive to large-scale production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1. By motile actinomycetes ( Actinoplanes deccanensis ) Mycelia fermented by SIIA-A2098 were leached with ethanol to obtain the crude extract of fidaxomicin. Weigh 5.0g of fidaxomicin crude product (fidaxomicin content is 47.2%) and dissolve in 150ml ethyl acetate by ultrasonic wave, and remove insoluble matter by filtration;

[0025] 2. Slowly add 50 ml of 0.5% sodium hydroxide solution by weight to the ethyl acetate phase and stir at 100-200 rpm for 20 minutes, then separate the phases with a tubular centrifuge. Collect the ethyl acetate phase and add 10 g of anhydrous sodium sulfate overnight. The ethyl acetate phase was obtained by filtration, and concentrated under reduced pressure;

[0026] 3. After the concentrate is dissolved, the sample is loaded onto a polyamide column (the filler is Polyammide-CC 6, the height-to-diameter ratio is 8.0, and the column volume is 100 ml), with 75% ethanol solution and 1.0% carbonic acid Gradient elution of mixed solvents of ...

Embodiment 2

[0031] 1. By motile actinomycetes ( Actinoplanes deccanensis ) Mycelia fermented by SIIA-A2098 were leached with ethanol to obtain the crude extract of fidaxomicin. Weigh 5.0 kg of fidaxomicin crude product (fidaxomicin content is 47.2% by weight respectively) and dissolve in 150L ethyl acetate by ultrasonic wave, and remove insoluble matter by filtration;

[0032] 2. Slowly add 50 liters of 0.5% sodium hydroxide solution by weight to the ethyl acetate phase and stir at 100-200 rpm for 20 minutes, then separate the phases with a tubular centrifuge. Collect the ethyl acetate phase and add 10 kg of anhydrous sodium sulfate overnight. The ethyl acetate phase was obtained by filtration, and concentrated under reduced pressure;

[0033] 3. After the concentrate is dissolved, the sample is loaded onto a polyamide column (the filler is Polyammide-CC 6, the aspect ratio is 8.0, and the column volume is 80 liters), with 75% ethanol solution by weight and 1.0% acetic acid by weight ...

Embodiment 3

[0038] 1. By motile actinomycetes ( Actinoplanes deccanensis ) Mycelia fermented by SIIA-A2098 were leached with ethanol to obtain the crude extract of fidaxomicin. Weigh 5.0 kg of fidaxomicin crude product (fidaxomicin content is 47.2% by weight respectively) and dissolve in 150L ethyl acetate by ultrasonic wave, and remove insoluble matter by filtration;

[0039] 2. Slowly add 50 liters of 1.5% sodium carbonate solution into the ethyl acetate phase and stir at 100-200rpm for 20 minutes, then use a tubular centrifuge to separate the phases. Collect the ethyl acetate phase and add 10 kg of anhydrous sodium sulfate overnight. The ethyl acetate phase was obtained by filtration, and concentrated under reduced pressure;

[0040]3. After the concentrate is dissolved, the sample is loaded onto a polyamide column (the filler is Polyammide-CC 6, the aspect ratio is 8.0, and the column volume is 80 liters), with 75% ethanol solution by weight and 0.5% formic acid by weight Gradient...

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PUM

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Abstract

The invention provides a method for separating and purifying fidaxomicin. The method solves the problems of a great number of separation steps, high production cost and low recovery rate of conventional methods for separating and purifying fidaxomicin. The method of the invention comprises the following steps: (1) dissolving a crude product containing fidaxomicin in an organic solvent, adding an alkali solution for washing, drying an organic phase with a drying agent, and then performing concentration under reduced pressure to obtain a concentrate; (2) allowing the concentrate obtained in thestep (1) to pass through a polyamide column, carrying out gradient elution, collecting an eluate containing fidaxomicin, and then performing concentration under reduced pressure and crystallization successively to obtain a white powdery pure product of fidaxomicin. The obtained fidaxomicin has a purity of 97% or more and total yield of 75% or more. The method of the invention can prepare high-purity fidaxomicin, has the advantages of fewer steps, simple and practicable process, high yield and environmental friendliness, and is very suitable for commercial production.

Description

technical field [0001] The invention relates to applications in the field of medicinal chemistry, in particular to a method for efficiently separating and purifying fidaxomicin. Background technique [0002] Fidaxomicin is a secondary metabolite produced by the fermentation of various microorganisms, also known as Tiacumicin B (Tiacumicin B), and its molecular formula is C 52 h 74 Cl 2 o 18 , It mainly inhibits bacterial RNA polymerase II to rapidly produce anti-refractory Clostridium infection (CDI), which is superior to existing drugs such as vancomycin and has a lower recurrence rate. [0003] Chinese invention patent CN104846043A discloses a method for preparing Fidaxomycin, which provides a process for separating and purifying Fidaxomycin from a fermentation broth, including: Dactylosporangium aurantiacum hamdenensis After the fermentation of the subspecies NRRL18085 strain, the mycelium was extracted with a polar organic solvent; the extract was concentrated and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08C07H1/06
CPCC07H1/06C07H17/08
Inventor 王欣荣翟龙飞褚以文傅慧垚张君利詹良静张新宜林家富刘超兰
Owner CHENGDU UNIV
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