Method for preparing mono-ammonium glycyrrhizinate
A technology of glycyrrhizic acid monoammonium salt and glycyrrhizic acid powder is applied in the directions of steroids, organic chemistry, etc., can solve problems such as high production cost, low product content, complicated process, etc., and achieves easy operation, high product content, and cost reduction. Effect
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Embodiment 1
[0009] Example 1: Take 1Kg of glycyrrhizic acid powder, add 6Kg of 95% ethanol for the first time to reflux for extraction at 50°C for 2 hours, filter and then add 8Kg of 95% ethanol, reflux for 2 hours, filter, then add 6Kg of 95% ethanol, reflux for 2 hours, and combine Add ammonia gas to the above filtrate until the pH value is between 5 and 6, stir for 1 h, let it stand for 24 h, and filter with suction to obtain the crude product of monoammonium glycyrrhizinate. After the solution is clear, add 25g of activated carbon, reflux for extraction for 1 hour, pour it out, let it stand for 12 hours, filter it with suction, and dry it in vacuum until the water content is 8%, to obtain the finished product of monoammonium glycyrrhizinate.
Embodiment 2
[0010] Example 2: Take 1Kg of glycyrrhizic acid powder, add 8Kg of methanol for the first time to reflux for extraction at 50°C for 2h, filter and then add 5Kg of methanol, reflux for 2h, filter, then add 5Kg of methanol, reflux for 2h, combine the filtrates, and feed ammonia gas , until the pH value is between 5 and 6, stir for 1h, let stand for 24h, and suction filter to obtain the crude product of monoammonium glycyrrhizinate. Add 6Kg of 85% ethanol to dissolve the monoammonium glycyrrhizinate. After the solution is clear, add 30g of activated carbon. Reflux for extraction for 1 hour, let stand for 12 hours, filter with suction, and vacuum-dry until the water content reaches 6%, to obtain the finished product of monoammonium glycyrrhizinate.
Embodiment 3
[0011] Example 3: Dissolve 1Kg of glycyrrhizic acid powder in a mixed solvent of 5Kg by weight of ethanol and acetone with a concentration of 90% and reflux 4 times, each time for 1 hour to obtain an extract. The mixture of ethanol and acetone is 1:1, and filter through 180um Cloth, combined filtrates, added ammonia gas to the obtained extract until the pH value was between 5 and 6 and stirred for 30min, then left to stand for 1h, passed through a 149um filter cloth, and the resulting precipitate was recrystallized with 4Kg of ethanol with a concentration of 75%. Once dried until the water content is below 8%, the monoammonium glycyrrhizinate is obtained.
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