Process for recovering steroids from residues in biological fermentation based androstenedione production

A technology of steroidal compounds and bio-fermentation, which is applied in the field of production of steroidal hormone raw material drugs, can solve the problems of large soil, water pollution, lower recovery rate, and warehouse occupation, so as to increase economic benefits, high recovery rate, The effect of reducing emissions

Inactive Publication Date: 2016-08-17
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

If it is not handled in time, it will not only reduce the recovery rate of androstenedione in the final refining section by about 15%, but also occupy the warehouse and cause a large

Method used

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  • Process for recovering steroids from residues in biological fermentation based androstenedione production
  • Process for recovering steroids from residues in biological fermentation based androstenedione production
  • Process for recovering steroids from residues in biological fermentation based androstenedione production

Examples

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Example Embodiment

[0029] Example 1

[0030] 5.0 g of solid scraps were taken, 15 mL of methanol was added, the temperature was raised to 50° C., stirred to reach a dissolution equilibrium, filtered, and the filter cake was dried to obtain steroid compound P1. Then concentrate the supernatant liquid, remove a part of methanol to obtain about 8 mL of supernatant liquid, slowly add water (about 8 mL) dropwise to it until the solution becomes a little cloudy, let stand for 1-24 h, separate layers, remove the lower oily matter by liquid separation, and separate the upper layer The emulsion was allowed to stand overnight, a solid was precipitated, filtered, and the filter cake was dried to obtain steroid P2. Methanol (10 mL) was first added to the lower layer of oil to dissolve, and then water (10 mL) was added to separate out the precipitate, which was filtered, and the filter cake was dried to obtain steroid compound P3. The combined products gave a pale yellow steroid (1.5 g). By HPLC analysis, ...

Example Embodiment

[0031] Example 2

[0032] Take 50.0 g of solid scraps, add 200 mL of ethanol, stir at room temperature to reach a dissolution equilibrium, filter, and dry the filter cake to obtain steroid compound P1. Then concentrate the supernatant liquid to remove a part of ethanol to obtain about 100 mL of supernatant liquid, to which water (about 120 mL) was slowly added dropwise until the solution appeared a little turbid, allowed to stand for 1-24 h, the layers were separated, the lower oily matter was removed by liquid separation, and the upper layer was separated. The emulsion was allowed to stand overnight, a solid was precipitated, filtered, and the filter cake was dried to obtain steroid P2. Ethanol (100 mL) was added to the lower layer of oil to dissolve, and then water (100 mL) was added to precipitate the precipitate, filtered, and the filter cake was dried to obtain steroid compound P3. The products were combined to give a pale yellow steroid (10.2 g). By HPLC analysis, the ...

Example Embodiment

[0033] Example 3

[0034] 5.0 g of solid waste was taken, 25 mL of ethyl acetate was added, the temperature was raised to 30° C., stirred to reach a dissolution equilibrium, filtered, and the filter cake was dried to obtain steroid compound P1. Then the supernatant liquid was concentrated, and a part of ethyl acetate was removed to obtain about 15 mL of supernatant liquid, to which cyclohexane (about 20 mL) was slowly added dropwise until the solution appeared a little turbid, left standing for 1-24 h, the layers were separated, and the lower layer was removed by liquid separation Oily matter, the upper layer of milky liquid was allowed to stand overnight, the solid was precipitated, filtered, and the filter cake was dried to obtain steroid compound P2. Ethyl acetate (20 mL) was added to the lower layer of oil to dissolve, and then cyclohexane (20 mL) was added to precipitate the precipitate, filtered, and the filter cake was dried to obtain steroid compound P3. The products ...

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Abstract

The invention relates to a method for recovering steroids from residues in biological fermentation based androstenedione production. The method includes steps: 1) dissolving solid residues in a solvent, heating and stirring until solubility equilibrium is achieved, filtering lower solids, drying to obtain solid steroids, concentrating supernatant, and removing part of the solvent to obtain clear liquid; 2) slowly adding the solvent into the clear liquid; stirring, standing, and performing liquid separation to remove lower oily substances to obtain upper emulsion; 3) standing the upper emulsion, filtering, and drying filter cakes to obtain the solid steroids; 4) dissolving the lower oily substances into the solvent to obtain clear liquid; 5) repeating the step 2) and the step 3), combining solids obtained each time with the solids obtained at the step 1) and the step 3) to obtain the steroids. The method has advantages that discharging quality of oily residues in biological fermentation based androstenedione production is reduced, environment pollution is relieved, and economic benefits of enterprises are increased.

Description

technical field [0001] The invention belongs to the technical field of production of steroid hormone raw material medicines, and in particular relates to a method for recovering steroidal compounds from leftovers of androstenedione produced by a biological fermentation method by using one or more mixed solvents. Background technique [0002] Androstenedione is an irreplaceable intermediate of steroid hormone drugs, and steroid hormone drugs are the second largest class of drugs after antibiotics in the world. For quite a long period of time, diosgenin was the main raw material for the synthesis of steroidal drugs, and more than two-thirds of the steroid hormone drugs in the world were produced based on diosgenin. Therefore, diosgenin has " "Mother of Hormones". Diosgenin mainly comes from turmeric, generally in the form of saponin, and saponin can be directly obtained by acid hydrolysis. Turmeric, also known as Dioscorea scutellaria, is highly selective to regions, and its...

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Application Information

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IPC IPC(8): C07J1/00C07J5/00
CPCC07J1/0011C07J5/0015
Inventor 池汝安徐彩丽张越非
Owner WUHAN INSTITUTE OF TECHNOLOGY
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