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A method for separating and purifying 11α-hydroxycanrenone

A hydroxycanrenone, separation and purification technology, applied in the directions of organic chemistry, steroids, etc., can solve the problems of cumbersome purification steps of 11α-hydroxycanrenone, and achieve the effects of high purity, simple procedure steps, and simple purification steps.

Inactive Publication Date: 2015-12-02
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This requires a large amount of toxic organic solvents, and the purification steps of 11α-hydroxycanrenone after extraction are cumbersome

Method used

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  • A method for separating and purifying 11α-hydroxycanrenone

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Experimental program
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Effect test

Embodiment 1

[0019] (1) Wash the Rhizopus slant covered with spores after culturing for 7 days with 15 mL of sterile water to obtain a spore suspension. Add 1mL of spore liquid into a 500mL Erlenmeyer flask containing 50mL of fresh sterile medium. After cultivating at 25°C and 220r / min for 48h, add canrenone so that the concentration of canrenone in the fermentation broth is 1g / L, continue After 48 hours of cultivation and transformation, the transformation rate was measured to be 91.3%, and the transformation was stopped. Among them: Rhizopus slant medium components include (g / L): glucose 22.0, yeast extract 20.0, soybean peptone 20.0, agar 30.0, adjust the pH of the medium to 5.0 with a 10% phosphoric acid solution; liquid transformation medium group Include (g / L): glucose 22.0, yeast extract 16.5, corn steep liquor 33.0.

[0020] (2) After centrifuging the converted fermentation broth at 1000 rpm for 30 minutes, the mycelium was dried at 40° C. and crushed to 200 mesh.

[0021] (3) Ex...

Embodiment 2

[0027] (1) Wash the slanted surface of Aspergillus ochrae that has been cultured for 5 days and is covered with spores with 5 mL of sterile water to obtain a spore suspension. Add 3mL of spore liquid into a 500mL Erlenmeyer flask containing 150mL of fresh sterile medium. After cultivating at 30°C and 150r / min for 24h, add canrenone so that the concentration of canrenone in the fermentation broth is 5g / L, continue After culturing and transforming for 96 hours, it was measured that the transformation rate was 96.2%, and then the transformation was stopped. Among them: Ochra slant medium components include (g / L): glucose 20.0, yeast extract 20.0, soybean peptone 20.0, agar 20.0, adjust the pH of the medium to 6.0 with a 10% phosphoric acid solution; liquid transformation medium group Include (g / L): glucose 20.0, yeast extract 25.0, corn steep liquor 2.0.

[0028] (2) After the transformed fermented liquid is subjected to vacuum filtration, the mycelium is dried at 100° C. and cr...

Embodiment 3

[0035](1) Wash the Rhizopus slant covered with spores after culturing for 5 days with 10 mL of sterile water to obtain a spore suspension. Add 2mL of spore liquid into a 500mL Erlenmeyer flask containing 100mL of fresh sterile medium. After culturing at 28°C and 200r / min for 36h, add canrenone so that the concentration of canrenone in the fermentation broth is 5g / L, continue After culturing and transforming for 84 hours, the transformation rate was measured to be 93.2%, and then the transformation was stopped. Among them: Rhizopus slant medium components include (g / L): glucose 22.0, yeast extract 20.0, soybean peptone 20.0, agar 30.0, adjust the pH of the medium to 5.0 with a 10% phosphoric acid solution; liquid transformation medium group Include (g / L): glucose 22.0, yeast extract 16.5, corn steep liquor 33.0.

[0036] (2) After centrifuging the converted fermentation broth at 6000 rpm for 10 minutes, the mycelium was dried at 80° C. and crushed to 100 mesh.

[0037] (3) Ex...

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Abstract

The invention relates to a method for separating and purifying 11α-hydroxycanrenone by using a macroporous resin, comprising mycelia separation, drying and crushing, heating alcohol extraction, adsorption separation and purification of a macroporous resin column, pressurized continuous chromatography, concentration and drying Dry. The technological process is simple, the cost is low, and the benefit is high. The chromatographic column can be activated and regenerated, and is suitable for industrial separation and purification of 11α-hydroxycanrenone. Heating and extracting with methanol solution can make the extraction rate of 11α-hydroxycanrenone higher. AB-8 macroporous resin can be used for continuous chromatography driven by a high-pressure constant-flow pump to obtain relatively pure 11α-hydroxycanrenone.

Description

technical field [0001] The patent of the present invention relates to a method for separating and purifying 11α-hydroxycanrenone by using a macroporous resin, and belongs to the field of extraction, separation and purification of microbial transformation products. Background technique [0002] 11α-Hydroxycanrenone is a steroid derivative formed after the hydroxylation reaction of canrenone, and it is also an important drug intermediate for the synthesis of eplerenone. As a new drug for the treatment of hypertension and other cardiovascular diseases, eplerenone has broad market prospects. The method for microbial conversion of canrenone to synthesize 11α-hydroxycanrenone has the advantages of strong specificity, mild reaction conditions, high catalytic efficiency, few by-products, low cost, and less pollution. [0003] Due to the extremely low solubility of 11α-hydroxycanrenone in water, 11α-hydroxycanrenone synthesized by microbial fermentation is mainly adsorbed on the sur...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J21/00
Inventor 管国强黄达明孙文敬崔凤杰崔鹏景钱静亚
Owner JIANGSU UNIV
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