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Method for extracting ergosterol from starch yeast

An ergosterol and starch fermentation technology, applied in the directions of steroids, organic chemistry, etc., can solve the problems of difficult three-waste treatment, insufficient market supply, cumbersome process steps, etc., and achieves less harmful impurities, less waste of resources, and short technological process. Effect

Inactive Publication Date: 2018-09-21
刘健
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process steps are cumbersome, there are many side reactions, the space-time yield is low, the three wastes are difficult to deal with, and the production cost is high, resulting in high product prices and insufficient market supply.

Method used

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  • Method for extracting ergosterol from starch yeast

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] (1) Saponification: Weigh 1kg of the fermented starch product, add it to a stirred container, add 1.2kg of ethanol, heat to maintain the temperature at 50-60°C, add 70g of potassium hydroxide, and stir for 16 hours. Then cool to room temperature.

[0049] (2) Filtration I: Ethanol is recovered by vacuum filtration.

[0050] (3) Extraction: Add the filter residue in step (2) into a stirred container, add 1.2 kg of ethyl acetate, heat to maintain the temperature at 50-60° C., and stir for 8 hours. Then cool to room temperature.

[0051] (4) Filtration II: vacuum filtration is used to collect the filtrate.

[0052] (5) Distillation: the filtrate collected in the step (4) is heated and distilled under normal pressure, and ethyl acetate is recovered by condensation. The residue was cooled to room temperature and filtered to obtain a light brown solid.

[0053] (6) Decolorization: Add the crystals obtained in step (5) into an airtight container, add 750 g of chloroform, s...

Embodiment 2

[0056] (1) Saponification: Weigh 5 kg of starch fermented product, add it to a stirring container, add 1.8 kg of methanol and 4.2 kg of methylene chloride; heat to maintain the temperature at 35-45°C, add 250 g of sodium hydroxide, and stir for 12 hours. Then cool to 25°C.

[0057] (2) Filtration I: Recover methanol and dichloromethane by vacuum filtration.

[0058] (3) Extraction: Add the filter residue in step (2) into a stirred container, add 5 kg of chloroform, heat to maintain the temperature at 50-60° C., and stir for 8 hours. Then cool to room temperature.

[0059] (4) Filtration II: vacuum filtration is used to collect the filtrate.

[0060] (5) Distillation: the filtrate collected in the step (4) is heated and distilled under normal pressure, and condensed to recover chloroform. The residue was cooled to room temperature and then filtered to obtain 4.7 g of crude ergosterol.

Embodiment 3

[0062] (1) Saponification: Weigh 1 kg of starch fermented product, put it into a stirred container, add 1.2 kg of methanol, heat to maintain the temperature at 50-55 ° C, add 50 g of sodium hydroxide, and stir for 18 hours. Then cool to room temperature.

[0063] (2) Filtration I: adopt vacuum filtration to recover methanol.

[0064] (3) Extraction: Add the filter residue in step (2) into a stirred container, add 1.2 kg of petroleum ether, heat to maintain the temperature at 40-50° C., and stir for 18 hours. Then cool to room temperature.

[0065] (4) Filtration II: vacuum filtration is used to collect the filtrate.

[0066] (5) Distillation: the filtrate collected in step (4) is heated and distilled under normal pressure, and petroleum ether is recovered by condensation. The residue was cooled to room temperature and then filtered to obtain a light brown ergot crude product.

[0067] (6) Decolorization: Add the crude product obtained in step (5) into an airtight container...

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Abstract

The invention belongs to the field of pharmaceutical intermediate and particularly discloses a method for extracting ergosterol from a starch yeast. The method comprises the following steps: (1) adding a solvent and a saponifying agent in the starch yeast containing the ergosterol to obtain to-be-filtered liquid I; (2) cooling and filtering the to-be-filtered liquid I; (3) adding an extracting agent in filter residues and stirring to obtain to-be-filtered liquid II; (4) cooling and filtering the to-be-filtered liquid II; (5) distilling a filtrate to obtain a crystal substance; (6) collecting the crystal substance, adding an extracting agent to re-dissolve, adding a coloring agent and stirring to obtain to-be-filtered liquid III; (7) filtering the hot to-be-filtered liquid III, collecting afiltrate and slowly cooling to precipitate out an ergosterol crude product; (8) adding a re-crystallization solvent in the collected ergosterol crude product, heating, then slowly reducing the temperature and collecting a crystal substance to obtain an ergosterol product. The method disclosed by the invention is short in short process; less in resource waste, resource-saving; high in product purity, less in harmful impurity and capable of environmental protection.

Description

technical field [0001] The invention belongs to the field of pharmaceutical intermediates, in particular to a method for extracting ergosterol from starch fermented products. Background technique [0002] Ergosterol is also known as ergosterol. Ergosterol is an important component of microbial cell membranes, and plays an important role in ensuring the integrity of cell membranes, the activity of membrane-bound enzymes, membrane fluidity, cell viability, and cell material transport. Ergosterol is a precursor for the production of vitamin D2 and an intermediate in the production of hormone drugs, which can be used to produce cortisone. It has the effect of vitamin D2. [0003] The traditional synthesis method of ergosterol is mainly based on microbial fermentation supplemented by traditional chemical synthesis and separation. The production process route is as follows: ERG9→squalene ERG1→epoxysqualene ERG7→lanosterol ERG11→4,4-dimethyl- Cholesta-8,14,24-trienol ERG24→4,4-d...

Claims

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Application Information

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IPC IPC(8): C07J9/00
CPCC07J9/00
Inventor 刘健潘桀李党辉吴路平
Owner 刘健
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