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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

AI Technical Summary

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 amount of pressure on the enterprise; Serious pollution of soil and water
At present, there is no literature report on the process of recycling steroidal compounds in this oily waste.

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

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Take 5.0 g of solid offal, add 15 mL of methanol, heat up to 50° C., stir to reach a dissolution equilibrium, filter, and dry the filter cake to obtain steroid compound P1. Then concentrate the supernatant, remove a part of methanol to obtain about 8mL of clear solution, slowly add water (about 8mL) dropwise thereto until the solution appears a little turbid, let it stand for 1-24h, separate layers, separate liquids to remove the lower oil, and remove the upper layer The emulsion was allowed to stand overnight, a solid precipitated out, filtered, and the filter cake was dried to obtain the steroidal compound P2. First add methanol (10 mL) to the oily substance in the lower layer to dissolve, then add water (10 mL) to precipitate a precipitate, filter, and dry the filter cake to obtain steroid compound P3. The products were combined to obtain a pale yellow steroid compound (1.5 g). Through HPLC analysis, the purity of androstenedione in the steroid compound is 75%, and ...

Embodiment 2

[0032] Take 50.0 g of solid waste, 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, remove a part of ethanol to obtain about 100mL of clear liquid, slowly add water (about 120mL) dropwise to it until the solution appears a little turbid, let it stand for 1-24h, separate layers, separate liquid to remove the lower oil, and remove the upper layer The emulsion was allowed to stand overnight, a solid precipitated out, filtered, and the filter cake was dried to obtain the steroidal compound P2. First add ethanol (100 mL) to the oily substance in the lower layer to dissolve, then add water (100 mL) to precipitate a precipitate, filter, and dry the filter cake to obtain steroid compound P3. The products were combined to obtain a light yellow steroid compound (10.2g). Through HPLC analysis, the purity of androstenedione in the steroid compound is 88%, an...

Embodiment 3

[0034] Take 5.0 g of solid offal, add 25 mL of ethyl acetate, heat up to 30° C., stir to reach a dissolution equilibrium, filter, and dry the filter cake to obtain steroid compound P1. Then concentrate the supernatant, remove a part of ethyl acetate to obtain about 15mL of clear liquid, slowly add cyclohexane (about 20mL) dropwise to it until the solution becomes slightly turbid, let it stand for 1-24h, separate layers, and remove the lower layer by liquid separation For oily matter, the upper milky liquid was left to stand overnight, and solids were precipitated, filtered, and the filter cake was dried to obtain steroidal compound P2. Ethyl acetate (20 mL) was first added to the oily substance in the lower layer to dissolve, then cyclohexane (20 mL) was added to precipitate a precipitate, filtered, and the filter cake was dried to obtain steroid compound P3. The products were combined to obtain a pale yellow steroid compound (1.3 g). Through HPLC analysis, the purity of andr...

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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...

Claims

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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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