Method of separating and extracting coenzyme Q10 from microbial fermentation broth
A microbial fermentation liquid, solid-liquid separation technology, applied in quinone separation/purification, organic chemistry, etc., to prevent dust from contaminating products, improve extraction yield, and increase the area of reaction contact
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Embodiment 1
[0046] Get 10L of rhodobacter sphaeroides fermented liquid (content is 3150mg / L), with Buchner funnel suction filter, the bacterial powder is dried in the vacuum oven, the bacterial powder after drying is pulverized to The particle size is about 2 μm, put it in a wide-mouth bottle, add 5 times the mass of n-hexane, stir and extract at about 30 ° C for 1 hour, the extract and bacterial residue are separated by a cyclone separator, the extract is passed through a silica gel column, and 4% of the Wash and elute with ethanol-n-hexane solution, collect the main section for concentration, recycle the solvent, add 2 times the mass of ethanol to the concentrate, heat to 60°C to dissolve, then cool down to 5°C at a rate of 5°C / h to crystallize , centrifuged, and dried to obtain 30.02 g of coenzyme Q10 finished product, with a purity of 99.60% and a total yield of 95.30%.
Embodiment 2
[0048] Get 10L of rhodobacter sphaeroides fermented liquid (content is 3150mg / L), with Buchner funnel suction filter, the bacterial powder is dried in the vacuum oven, the bacterial powder after drying is pulverized to The particle size is about 5 μm, put it in a jar, add 10 times the mass of ether, stir and extract at about 40 ° C for 1.5 hours, the extract and fungal residue are separated by a cyclone separator, the extract is passed through a silica gel column, and 10% Wash and elute with methyl acetate-methanol solution, collect the main section for concentration, recycle the solvent, add 4 times the mass of acetone to the concentrate, heat to dissolve, then cool down to 10°C at a rate of 10°C / h to crystallize, centrifuge Filter and dry to obtain 30.53g of coenzyme Q10 finished product with a purity of 99.61% and a total yield of 96.92%.
Embodiment 3
[0050] Get 10L of rhodobacter sphaeroides fermented liquid (content is 3150mg / L), with Buchner funnel suction filter, the bacterial powder is dried in the vacuum oven, the bacterial powder after drying is pulverized to The particle size is about 10 μm, put it in a jar, add 15 times the quality of petroleum ether, stir and extract at about 35 ° C for 1.2 hours, the extract and fungus residue are passed into a cyclone separator for separation, the extract is passed through a silica gel column, and 15% The butanone-n-heptane solution was washed and eluted, the main section was collected and concentrated, the solvent was recycled, and 8 times the mass of ethanol was added to the concentrate, heated to 55°C to dissolve, and then cooled at a rate of 12°C / h to Crystallized at 15°C, centrifugally filtered, and dried to obtain 30.72 g of finished coenzyme Q10 with a purity of 99.67% and a total yield of 97.52%.
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