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Method for preparing hydroginkgolic acid
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A hydrogenated ginkgoic acid and drying technology, applied in the separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problems of serious pollution, low content of hydrogenated ginkgoic acid, unfavorable large-scale production operations, etc.
Inactive Publication Date: 2010-05-12
SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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[0005] In the prior art, the extraction and separation method of hydrogenated ginkolic acid mainly adopts organic solvent method, etc., but the content of hydrogenated ginkolic acid obtained by these extraction processes is low, the pollution in the production process is serious, and it is unfavorable for large-scale production operations
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Embodiment 1
[0015] Get 10Kg of dry ginkgo fruit coarse powder, add 50% ethanol to percolate, collect the percolation liquid of 5 times of volume of its weight, filter, reclaim ethanol under reduced pressure and concentrate, filter, filtrate passes styrene strong acid cation exchange resin , water elution to remove impurities, 1mol / L NaOH elution, each column volume of the eluent as a fraction, collect the eluent from the 5th fraction to the 10th fraction, combine, concentrate, place, and crystallize, The crystals were separated, recrystallized by adding methanol, separated, washed and dried to obtain 6.1 g of hydrogenated ginkgoic acid, which was detected by HPLC with a purity of 98.2%.
Embodiment 2
[0017] Take 10Kg of dried ginkgo fruit powder, add 80% ethanol for percolation, collect the percolation liquid with 12 times the volume of its weight, filter, recover ethanol under reduced pressure and concentrate, filter, the filtrate passes through weak acid cation exchange resin, and washes with water Removal of impurities, elution with 1mol / L NaOH, the eluent of each column volume is regarded as one fraction, the eluent from the 5th fraction to the 10th fraction is collected, combined, concentrated, placed, crystallized, separated and crystallized , adding methanol for recrystallization, separation, washing, and drying to obtain 9.2 g of hydrogenated ginkgoic acid, which was detected by HPLC with a purity of 98.6%.
Embodiment 3
[0019] Take 10Kg of dry ginkgo fruit powder, add 70% ethanol for percolation, collect the percolation liquid of 8 times the volume of its weight, filter, recover ethanol under reduced pressure and concentrate, filter, and the filtrate passes through phenolsulfonic acid type strong cation exchange Resin, eluted with water to remove impurities, eluted with 1mol / L NaOH, the eluate of each column volume is regarded as a fraction, the eluate from the 5th to the 10th fraction is collected, combined, concentrated, placed, and crystallized , separated and crystallized, added methanol for recrystallization, separated, washed and dried to obtain 11.2 g of hydrogenated ginkgoic acid, which was detected by HPLC with a purity of 99.4%.
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Abstract
The invention relates to a method for preparing hydroginkgolic acid, which has simple and convenient operation, light pollution, and less equipment investment. The method comprises the following process steps: adding 50 to 80 percent ethanol into dry ginkgofructification coarse powder for seeping, and collecting percolate of which the weight is 5 to 12 times weight of the dry ginkgofructification coarse powder; filtering the percolate, recovering the ethanol at reduced pressure, concentrating, filtering, passing the filter liquor through a cation exchange resin, eluting with water to remove impurities, and eluting with 1mol / L NaOH; and taking each column volume of eluent as a flow part, collecting eluent from the fifth flow part to the tenth flow part, merging the eluent, concentrating, standing and crystallizing the eluent, performing fractional crystallization, and adding ethanol for recrystallization. The hydroginkgolic acid prepared by the method has high purity, and industrial enlargement is easy to realize.
Description
technical field [0001] The invention relates to a preparation method of hydrogenated ginkolic acid, in particular to a method for extracting hydrogenated ginkolic acid from plants. Background technique [0002] Hydroginkgolic acid, molecular formula: C 22 h 36 o 3 , molecular weight: 348.525, CAS accession number: 16611-84-0, the structural formula is as follows: [0003] [0004] Hydrogenated ginkgoic acid is a natural compound that has physiological activities such as relieving cough and reducing phlegm, and is mainly found in the fruit of Ginkgo biloba, a plant of the Ginkgo family. [0005] In the prior art, the extraction and separation method of hydrogenated ginkolic acid mainly adopts organic solvent method, etc., but the content of hydrogenated ginkolic 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 tec...
Claims
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