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
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[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, ...
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[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 ...
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[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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