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A method for extracting 4-androstenedione from phytosterol fermentation broth

A technology of phytosterols and androstenedione, which is applied in the direction of steroids and organic chemistry, can solve the problems of short extraction steps, long purification steps, and many types of solvents, and achieves short process routes, fewer types of solvents, and reduced Effect of Raw Materials and Solvent Costs

Inactive Publication Date: 2015-09-30
SHANDONG DONGYAO PHARMACEUTICAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The technical problem to be solved by the present invention is to overcome the shortcomings of many kinds of solvents used and long purification steps in the existing technology, and design a kind of extraction step with short extraction steps, high product yield, high content, and unreacted starting raw material phytosterols that can be recovered and reused. The extraction method used

Method used

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  • A method for extracting 4-androstenedione from phytosterol fermentation broth
  • A method for extracting 4-androstenedione from phytosterol fermentation broth

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Embodiment Construction

[0036] (1) 100L of fermented liquid was filtered through a plate and frame filter press to obtain a wet filter cake of about 25kg, containing 10% of 4-androstenedione (4-AD); extracted three times with acetone, and the first time with acetone 37.5 L, leaching for 2 hours, the second time using acetone 25L, leaching for 1.5h, the third time using acetone 20L, leaching for 1.5h, combining the three extracts to about 82.5L, standing at 4°C for 5h, centrifuging to collect the filtrate and The unreacted phytosterol was about 2.5kg, and the filtrate was evaporated under reduced pressure to recover acetone, cooled to 4°C to grow crystals for 3 hours, and centrifuged to obtain about 3.38kg of crude 4-androstenedione (I); crude 4-androstenedione (I) Dissolve the crude product in 47.3L of 50% acetone aqueous solution, heat to reflux, filter, and the filtrate is cooled to 4°C and stirred for 3 hours to crystallize, and centrifuged to obtain about 2.51kg of the crude product of 4-androsten...

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Abstract

The invention discloses a method of extracting 4-androstenedione from plant sterol fermentation liquor. Particularly, 4-androstenedione crude products (I) and unreacted plant sterol are extracted from mycelium and slag charges which are separated from the fermentation liquor and soaked by acetone; the 4-androstenedione crude products (I) are dissolved and crystallized by acetone aqueous solution with a concentration of 50% so that crude products (II) are obtained; and the crude products (II) are recrystallized by alcohol so that pure 4-androstenedione is obtained, wherein the ratio of the alcohol to water is 1:10, and the unreacted plant sterol is recrystallized by the alcohol so that recovered plant sterol is obtained, wherein the ratio of the alcohol to water is 1:10. The method of extracting the 4-androstenedione from the plant sterol fermentation liquor is good in extraction effect, high in product purity, easy to operate, few in number of types of solvents used, capable of reducing environmental pollution, low in cost, short in process route and suitable for industrialized production. The unconverted plant sterol can be recovered and recycled.

Description

technical field [0001] The invention relates to a method for extracting 4-androstenedione (4-AD) from phytosterol fermentation liquid, belonging to the technical field of biological fermentation extraction. Background technique [0002] 4-Androstenedione (4-AD) is an intermediate in the synthesis of various hormone APIs. Its production method is biotransformation of phytosterols through special bacterial fermentation, and a small amount of androstenedione is also produced during the fermentation process. (ADD), therefore, 4-androstenedione (4-AD), androstenedione (ADD) and unreacted phytosterols exist in the fermentation broth at the same time, and their solubility differences in solvents are not obvious, Separation and purification are difficult, and the existing extraction process is complicated. After more than 4 extractions and with multiple solvents, the product content is low, and multiple solvents cause serious environmental pollution. Contents of the invention [...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J1/00
Inventor 郭锋杨永芝孟强王凤滩于新令
Owner SHANDONG DONGYAO PHARMACEUTICAL CO LTD
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