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Preparation method for sirolimus coarse crystal

A technology of sirolimus and rolimus bacteria, which is applied in the field of preparation of coarse crystals of sirolimus, can solve problems such as not seen, and achieve the effects of simple operation, improved purity and content, and increased ratio

Active Publication Date: 2012-03-14
FUJIAN INST OF MICROBIOLOGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The invention provides a method for preparing sirolimus coarse crystals without complicated procedures, and there is no product in the form of sirolimus coarse crystals currently on the market

Method used

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  • Preparation method for sirolimus coarse crystal
  • Preparation method for sirolimus coarse crystal

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preparation example Construction

[0021] A method for preparing sirolimus coarse crystals, firstly filtering sirolimus fermentation broth, then removing the supernatant to obtain sirolimus mycelia, and then extracting sirolimus mycelium with alcohol to obtain Extract of sirolimus mycelium. The extract of sirolimus mycelia is operated in the following steps:

[0022] (1) Adsorption: Concentrate the extract of sirolimus mycelium into a concentrate under reduced pressure, then add a solid adsorbent to the concentrate, stir, let stand, and then decant to remove the liquid to obtain a residue, wherein, The amount of solid adsorbent to be added is based on the volume of the extract, and 0.001-0.005 kg of solid adsorbent is added per liter of extract, and the solid adsorbent is one or more of diatomaceous earth and silica gel.

[0023] (2) Extraction: add 0.05 to 0.5 times the volume of the leaching solution to the residue obtained from the treatment in (1), stir, then filter or centrifuge to remove the solid, and t...

Embodiment 1

[0030] A method for preparing sirolimus coarse crystals, the extract of sirolimus mycelia is operated by the following steps:

[0031] (1) Adsorption: Concentrate 100 L of sirolimus mycelium extract under reduced pressure into a concentrate, then add 0.1 kg of solid adsorbent diatomaceous earth to the concentrate, stir, let stand, then pour to remove the liquid To obtain a residue, the purpose of the solid adsorbent used in the present invention is to adsorb impurities in the concentrate.

[0032] (2) Extraction: Add 5L of ethyl acetate to the residue obtained from (1) treatment, and stir, then filter or centrifuge to remove the solid, then leave the resulting solution to separate the solution into two layers of water and organic solution, And the aqueous layer was removed to obtain an organic solution.

[0033](3) Washing and concentration: add saturated brine 0.1 times the volume of the above organic solution to the organic solution obtained through (2) treatment, wash the ...

Embodiment 2

[0040] This part differs from Example 1 in that:

[0041] (1) Adsorption: 0.5Kg of solid adsorbent silica gel is added to the concentrate; (2) Extraction: 50L of dichloromethane is added to the residue obtained from (1) treatment; (3) Washing and concentration: adding the volume of the above organic solution Equal saturated saline into the organic solution obtained through (2) treatment; (4) washing: add non-polar solvent hexane 3 times the volume of the above-mentioned oily substance to the oily substance obtained through (3) treatment; (5 ) Crystallization: adding 3 times the volume of the above residue as a crystallization solvent methyl tert-butyl ether to the residue obtained from the treatment in (4), then placing the sirolimus solution at room temperature for 10 h; (6) washing the crystal Drying: wash the sirolimus crystal obtained in (5) with the crystallization solvent methyl tert-butyl ether three times; (7) detection: the purity of sirolimus reaches 97.8%, isomer B:...

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Abstract

The invention provides a preparation method for a sirolimus coarse crystal. The method comprises adsorbing, extracting, washing, concentrating, crystallizing, washing a crystal, drying and the like to obtain the sirolimus coarse crystal. In the preparation method, a series of complicated processes such as column chromatography and the like are not required, the sirolimus coarse crystal can be obtained through simple and conventional experimental operation, the operation is simple, and industrial production can be performed. Due to the adoption of the preparation method, the purity and the content of the sirolimus coarse crystal are greatly increased, and the ratio of an isomer B to an isomer C in sirolimus is increased. At present, a product of sirolimus existing in the form of coarse crystal is not commercially available. The sirolimus coarse crystal prepared with the method has the advantage of convenience for storing and transporting, and great convenience is brought to a large quantity of research personnel or production personnel.

Description

【Technical field】 [0001] The invention relates to a preparation method of medicine, in particular to a preparation method of sirolimus coarse crystal. 【Background technique】 [0002] Sirolimus (sirolimus), also known as rapamycin (rapamycin), was first obtained in 1975 from the Streptomyees hygroscopicus fermentation broth isolated from the soil samples of Pacific Easler Island by Vezina et al. . Sirolimus is a lipophilic nitrogen-containing 36-membered macrolide antibiotic with the molecular formula C 51 h 79 NO 13 , molecular weight 914.2, its structural formula is as follows: [0003] [0004] In 1977, Morris et al. first discovered that sirolimus had immunosuppressive effects, and began to use sirolimus as a new drug for the treatment of organ transplant rejection in 1989. It is the latest powerful immunosuppressant in the world, its immunosuppressive activity is dozens of times stronger than cyclosporine widely used in clinical practice, not only has low toxicit...

Claims

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Application Information

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IPC IPC(8): C07D498/18
Inventor 杨国新程元荣黄捷余辉金东伟陈夏琴陈有钟
Owner FUJIAN INST OF MICROBIOLOGY