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Method for extracting androstenedione in bi-liquid phases system

An androstenedione, two-phase technology, applied in steroids, organic chemistry and other directions, can solve the problems of large solvent consumption, low product content, environmental pollution, etc., and achieves reduction of solvent types, convenient production and operation, and removal of impurities. Effect

Inactive Publication Date: 2015-06-17
SHANDONG FANGMING PHARMACEUTICAL CO LTD
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

In recent years, the production of steroidal drugs has continued to grow, and the processing industry of synthetic steroidal drugs using phytosterols as raw materials has risen rapidly, but a small amount of androstenedione (ADD) is also produced during the fermentation process. Therefore, 4-androstenedione ( 4-AD), androsdienedione (ADD) and unreacted phytosterols exist in the fermentation broth at the same time, and their solubility differences in solvents are not obvious, and separation and purification are difficult. The existing extraction process is complicated and the solvent consumption is large. , low product content, serious environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0019] (1) Fermentation broth pretreatment

[0020] Take 50L of two-phase fermentation broth, heat it to 90°C, stir for 15min, let it stand for 1h, drain the lower water phase, collect 18L of the upper emulsified layer (4-AD content 3.79%), concentrate under reduced pressure at 60°C, and evaporate to dryness water, 12.5L of concentrated emulsified layer (4-AD content 5.42%) was obtained.

[0021] (2) Methanol extraction

[0022] Add 50 L of methanol to 12.5 L of the above-mentioned concentrated emulsified layer, stir for 1.5 h, and let the layers stand for 1 h. The upper methanol phase was collected for use (4-AD content 10.16g / L), the lower oil phase was stirred with 38L methanol for 1.5h, allowed to stand for more than 1h, and the upper methanol phase was collected (4-AD content 4.37g / L), the lower layer The oil phase was discarded. The two methanol phases were combined, and the layers were allowed to stand for 20 min to separate the residual oil phase.

[0023] (3) Extr...

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Abstract

The invention discloses a method for extracting androstenedione in a bi-liquid phases system. which is characterized in that a broth is pretreated, and is extracted by methanol and is performed with vacuum concentration until no methanol is generated, and then filtered to obtain a crude product I, washing the crystal by a mixing solvent to obtain a crude product II, and the crude product II is performed through twice methanol purification and dried to obtain the androstenedione pure product. The method has the advantages of good extraction effect and high product purity, methanol is taken as a main solvent, the cost is low, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for extracting androstenedione from a two-liquid phase system, belonging to the technical field of fermentation separation and extraction. Background technique [0002] Androstenedione (4-AD) is an important intermediate in the synthesis of various hormone drugs, which can be used to produce more than 100 kinds of drugs such as sex hormones, progestins, and anabolic hormones, and plays a very important role in regulating the body. In recent years, the production of steroidal drugs has continued to grow, and the processing industry of synthetic steroidal drugs using phytosterols as raw materials has risen rapidly, but a small amount of androstenedione (ADD) is also produced during the fermentation process. Therefore, 4-androstenedione ( 4-AD), androsdienedione (ADD) and unreacted phytosterols exist in the fermentation broth at the same time, and their solubility differences in solvents are not obvious, and separation an...

Claims

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Application Information

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IPC IPC(8): C07J1/00
CPCC07J1/0011
Inventor 赵昂袁国良牛宏彦于新令刘祎祯程传东
Owner SHANDONG FANGMING PHARMACEUTICAL CO LTD
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