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A technique of scholastic acid and shironic acid, which is applied in the field of preparation of shironic acid, and can solve problems such as unfavorable large-scale production operations, low shironic acid content, serious pollution and the like
Inactive Publication Date: 2010-05-12
SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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[0005] In the prior art, the extraction and separation methods of pulicic acid mainly adopt organic solvent method, etc., but the content of pulicic acid ob
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Embodiment 1
[0016] Take 10Kg of agaric powder, add 60% ethanol which is 5 times the volume of its weight, heat and reflux once, each time for 1 hour, combine the reflux liquid, filter, recover the ethanol under reduced pressure and concentrate, add an equal volume of acetone to extract 3 times, and combine For the acetone layer, recover the solvent and concentrate, add an equal volume of water and stir evenly, let it stand overnight, filter, take the filter residue, add acetone-ethanol (1:1) to crystallize, separate the crystals, wash and dry to obtain 258.2 g of pharylic acid. As detected by HPLC, the purity is 98.3%.
Embodiment 2
[0018] Take 10Kg of Tremella auricularia powder, add 90% ethanol 10 times the volume of its weight, heat and reflux 3 times, 3 hours each time, combine the reflux liquid, filter, recover ethanol under reduced pressure and concentrate, add an equal volume of acetone to extract 7 times, and combine For the acetone layer, recover the solvent and concentrate, add an equal volume of water and stir evenly, let stand overnight, filter, take the filter residue, add acetone-ethanol (1:1) to crystallize, separate the crystals, wash, and dry to obtain 289.4 g of strialic acid. HPLC detection, the purity is 98.0%.
Embodiment 3
[0020] Take 10Kg of Tremella auricularia powder, add 80% ethanol with 8 times the volume of its weight, heat and reflux twice, each time for 2 hours, combine the reflux liquid, filter, recover ethanol under reduced pressure and concentrate, add an equal volume of acetone to extract 5 times, and combine For the acetone layer, recover the solvent and concentrate, add an equal volume of water and stir evenly, let it stand overnight, filter, take the filter residue, add acetone-ethanol (1:1) to crystallize, separate the crystals, wash and dry to obtain 308.2 g of pharylic acid. As detected by HPLC, the purity is 99.6%.
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Abstract
The invention relates to a preparation method for a gyrophoric acid, which has simple and convenient operation, little pollution and less equipment investment. The preparation method comprises the following processing steps: taking coarse gyrophora powder; adding 60 to 90 percent ethanol of which the weight is 5 to 10 times that of the volume; heating and refluxing a mixture of the gyrophora powder and the ethanol for 1 to 3 times, 1 to 3 hours for each time; amalgamating refluxed liquids; filtering an amalgamated liquid; recycling the ethanol under a reduced pressure and concentrating the recycled ethanol; adding acetone of an equal volume to extract 3 to 7 times; amalgamating acetone layers; recycling and concentrating a solvent; adding water of the equal volume and stirring the mixture uniformly; standing the mixture over night; filtering the mixture; taking filter residue; and adding acetone-ethanol (1:1) to crystallize. Due to the adoption of the preparation method for the gyrophoric acid, the product purity is high, and industrialization enlargement is easy to realize.
Description
technical field [0001] The present invention relates to a preparation method of pyrophyllic acid, in particular to a method for extracting pyrophyllic acid from plants. Background technique [0002] Gyrophoric acid, molecular formula: C 24 h 20 o 10 , molecular weight: 468.416, CAS accession number: 548-89-0, the structural formula is as follows: [0003] [0004] Pulmonic acid is a natural compound with physiological activities such as anti-ATP synthesis, mainly found in plants such as Umbllicaria esclenta (Miyoshi) Minks. [0005] In the prior art, the extraction and separation methods of pulicic acid mainly use organic solvent methods, etc., but the content of pulicic acid obtained by these extraction processes is low, the pollution in the production process is serious, and it is not conducive to large-scale production operations. Contents of the invention [0006] The technical problem to be solved by the present invention is to provide a method for preparing pu...
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