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Preparation method of fidaxomicin crystal

A technology for fidaxomicin and crystals, applied in the field of preparation of fidaxomycin crystals, can solve problems such as limiting industrial application, increasing production cost, adverse environmental impact, etc., achieving low cost, avoiding human injury, and solvent dosage. less effect

Active Publication Date: 2013-09-04
NCPC NEW DRUG RES & DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method is simple to operate, it takes a long time to crystallize and is time-consuming and labor-intensive.
Most of the solvents used in this method are the second-class solvents stipulated by the International Conference on Harmonization (ICH), which will have a great adverse impact on the environment, and the amount of solvents used is large, resulting in waste of solvents, increased production costs, and limited its industrialization. application

Method used

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  • Preparation method of fidaxomicin crystal
  • Preparation method of fidaxomicin crystal

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preparation example Construction

[0020] Preparation of Fidaxomycin fine powder:

[0021] Take 10 liters of fidaxomicin fermentation broth, and the fermentation unit is 510 micrograms / ml. The fidaxomicin fermentation broth was filtered to obtain 2.5 kg of mycelia. Add 5 liters of 80% methanol aqueous solution to the above-mentioned mycelia, stir and extract for 1 hour, then filter, and collect the fidaxomicin extract. The extract was diluted with water to a methanol concentration of 30%, and then introduced into a macroporous resin LX98 column for decolorization. The resin loading capacity was 500 ml, and the flow rate was 1000 ml / hour. The decolorization solution is introduced into the macroporous resin HZ816 column again for adsorption, the resin loading capacity is 500 milliliters, and the flow rate is 1000 milliliters / hour. The saturated resin was desorbed successively with 40% and 80% methanol aqueous solution at a flow rate of 500 ml / hour, and the desorption solution was collected in sections. The fid...

Embodiment 1

[0023] Take 20 grams of fidaxomicin, heat and dissolve it with 600 ml of 60% ethanol aqueous solution at 45°C, cool to 0°C and crystallize for 24 hours after the dissolution is complete, perform vacuum filtration after crystallization, and place the filter cake in an oven at 45°C After vacuum drying for 2 hours, 15.2 g of fidaxomicin crystals were obtained, with a yield of 76%. The XRPD pattern of the made Fidaxomycin crystal is as follows figure 1 shown.

Embodiment 2

[0025] Take 20 grams of fidaxomicin and dissolve it with 200 ml of 70% ethanol aqueous solution under heating at 40°C. After the dissolution is complete, cool to 20°C for crystallization for 48 hours. Vacuum drying in an oven for 3 hours yielded 16 g of fidaxomicin crystals, with a yield of 80%.

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Abstract

The invention discloses a fidaxomicin crystal and a preparation method of the crystal. Characteristic peaks, expressed by 2 theta, of an X-ray powder diffraction spectrum of the crystal are located at 3.324, 7.745, 9.989, 1.607, 13.954, 14.475, 15.355, 15.855, 18.800, 19.999, 20.321, 22.245, 23.104, 24.028 and 24.446. The method comprises the preparation steps of dissolving fidaxomicin in an aqueous solution of alcohol, crystallizing, conducting suction filtration, drying, and obtaining the fidaxomicin crystal. The preparation method has the advantages that the preparation method is stable in process and simple and quick to operate, facilitates environmental protection, and is appropriate to industrial production. The obtained fidaxomicin is stable in crystal form and uniform in particle, and facilitates subpackage and storage.

Description

technical field [0001] The invention relates to a method for preparing compound crystals, more precisely, relates to a method for preparing fidaxomicin crystals. Background technique [0002] Fidaxomicin is a new macrolide antibiotic with an 18-membered ring structure produced by the fermentation of D. aurantiacus. It is mainly resistant to Gram-positive aerobic and anaerobic bacteria, Clostridium difficile, and also has good antibacterial effect on methicillin-resistant Staphylococcus aureus, Clostridium perfringens and Enterococcus. Fidaxomicin is mainly used clinically for the treatment of diseases caused by Clostridium difficile infection. It has the advantages of low tendency to develop resistance, long-lasting post-antibiotic effect, low cross-resistance and few adverse reactions. [0003] [0004] Fidaxomycin is a polymorphic compound, usually in the form of white needle-like, snowflake-like crystals or amorphous powder, easily soluble in methanol, ethanol, ethyl ...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/06
Inventor 任风芝张雪霞段宝玲王海燕陈书红李晓露胡卫国
Owner NCPC NEW DRUG RES & DEV
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