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Method for recovering and refining androstenedione from the solid waste of androstenedione prepared by microbial method

A technology of androstenedione and microorganism method is applied in the field of synthesis and separation of pharmaceutical intermediates, which can solve the problems of complex composition of compounds, ineffective utilization of compounds, ineffective utilization of steroid compounds, etc., so as to reduce the risk of environmental pollution, The effect of improving economic efficiency

Active Publication Date: 2020-01-14
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, after microbial degradation of phytosterols, not only C-17 intermediates are obtained, but also a large amount of leftovers are left. These leftovers have not been effectively utilized at present. How to efficiently recover androstenedione has become an urgent problem to be solved.
[0004] Chinese patent CN105859813A reports a process for recovering steroidal compounds from the leftovers of androstenedione produced by biological fermentation. The method uses a variety of mixed solvents to recover steroidal compounds from the leftovers of androstenedione produced by microbial methods , but the components of the recovered compounds are complex, and some of the more important steroidal compounds have not been separated, and the separated steroidal compounds cannot be used effectively

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The first step: take 5g of the solid offal of androstenedione prepared by microbial method and place it in a beaker, add 100mL of toluene to it, heat to 40°C and stir for 1h, and filter after it reaches equilibrium after dissolving for 3h to obtain the supernatant and Insoluble solid material in the lower layer.

[0025] Step 2: Dry the insoluble solid substance in the lower layer in the previous step, then add 20 mL of acetone, heat to 40°C and stir for 1 hour, and filter after dissolving for 2 hours to reach equilibrium to obtain the supernatant liquid and the insoluble solid substance in the lower layer.

[0026] The third step: drying the insoluble solid matter in the lower layer of the previous step, repeating the first step and the second step twice each, and the finally obtained insoluble solid matter is a steroid compound and a fat solid compound.

[0027] Step 4: Combine the supernatants in the above steps and concentrate under reduced pressure to obtain a colo...

Embodiment 2

[0031] The first step: take 20g of the solid waste of androstenedione prepared by the microbial method and put it in a beaker, add 250mL of petroleum ether to it, heat to 60°C and stir for 2h, wait for it to dissolve for 0.5h to reach equilibrium and filter to obtain the supernatant liquid and the lower layer of insoluble solid matter.

[0032] The second step: dry the insoluble solid substance in the lower layer obtained in the previous step, then add 90mL of ethyl acetate, heat to 60°C and stir for 1 hour, and filter after dissolving for 2 hours to reach equilibrium to obtain the supernatant liquid and the insoluble solid substance in the lower layer.

[0033] The third step: drying the insoluble solid substance in the lower layer obtained in the previous step, and repeating the first step and the second step 3 times respectively, and the finally obtained solid insoluble substance is steroidal compound and fat solid compound.

[0034] Step 4: Combine the supernatants in the ...

Embodiment 3

[0038] The first step: take 100g of the solid waste of androstenedione prepared by microbial method and put it in a beaker, add 800mL of dichloromethane into it, heat to 20°C and stir for 1h, wait for it to dissolve for 1h and reach equilibrium for 1h, then filter to obtain the upper layer supernatant and lower layer of insoluble solid matter.

[0039] The second step: dry the insoluble solid substance in the lower layer obtained in the previous step, then add 20 mL of benzene, heat to 50° C. and stir for 1 hour, and filter after 3 hours of dissolving to reach equilibrium to obtain the supernatant liquid and the insoluble solid substance in the lower layer.

[0040] The third step: drying the insoluble solid substance in the lower layer obtained in the previous step, repeating the first step and the second step each once in a cycle, and the finally obtained solid insoluble substance is a steroid compound and a fat solid compound.

[0041]Step 4: Combine the supernatants in the...

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Abstract

The invention relates to a method for recycling and refining androstenedione from solid leftovers produced during preparation of the androstenedione by a microbial method. The method comprises the following steps: repeatedly dissolving and separating solid insolubles in the leftovers by using different types of solvents, finally combining filtrates, concentrating, and then performing separating purification to obtain the androstenedione of high purity and good yield. By the method, effective separation and recycling of waste leftover resources are achieved, the risk of environment pollution isreduced and the economic benefits of an enterprise are increased.

Description

technical field [0001] The invention relates to the technical field of synthesis and separation of pharmaceutical intermediates, in particular to a method for recovering and refining androstenedione from the solid waste of androstenedione prepared by a microbial method by using a mixed solvent and column chromatography analysis technology. Background technique [0002] Steroid hormones are widely used clinically as the second largest class of drugs next to antibiotics. As raw materials for the preparation of various steroid drugs, steroid hormone intermediates are widely used and of various types, and have important medical value and huge market demand. The production methods of steroid hormone intermediates mainly include saponin method and sterol method. The saponin method uses saponin as a raw material, and after esterification, cracking, oxidation, and hydrolysis, acetic acid gestational dienolone (abbreviated as diene) is obtained, and the diene is then synthesized int...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J1/00
CPCC07J1/0011
Inventor 肖春桥池汝安陶琪
Owner WUHAN INSTITUTE OF TECHNOLOGY