Preparation method of pectolinarin reference substance
A technology for crude fish leaf glycosides and fish leaf glycosides, which is applied in the field of modernization of traditional Chinese medicine, and can solve problems such as poor solubility of fish leaf glycosides, difficulty in separating monomers, and insufficient supply
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Embodiment 1
[0059] The preparation method of the leaf glucoside reference substance of Liu Chuanyu is characterized in that it is carried out according to the following process steps:
[0060] A. Raw material extraction: add 180L ethanol solution with a volume fraction of 70% to 30Kg of thistle medicinal material, heat extraction at 60°C for 2 times, each time for 2 hours, cool to room temperature, filter with suction, combine filtrates, concentrate to no alcohol Flavor, 10L in total;
[0061] B. Macroporous resin enrichment: Weigh 6KgAB-8 macroporous adsorption resin and pack it into a column, statically adsorb the concentrated solution of step A with macroporous resin for 15 hours overnight, and then use 30% of 25L water and 20L column volume respectively Elute the impurities with ethanol solution, then elute the target substance with 10L of 60% ethanol solution, collect the eluent, and concentrate to 400ml;
[0062] C. Polyamide purification: add 3% NaOH solution to the concentrated s...
Embodiment 2
[0069] A. Raw material extraction: Add 100Kg of thistle medicinal material, add 600L ethanol solution with a volume fraction of 70%, heat extraction at 60°C for 2 times, each time for 2 hours, cool to room temperature, filter with suction, combine the filtrates, and concentrate to no alcohol Flavor, 30L in total;
[0070] B. Macroporous resin enrichment: Weigh 20KgAB-8 macroporous adsorption resin and pack it into a column, statically adsorb the concentrated solution of step A with macroporous resin for 15 hours overnight, and then use 30% of 80L water and 50L column volume respectively Elute the impurities with ethanol solution, then elute the target substance with 30L of 60% ethanol solution, collect the eluent, and concentrate to 1000ml;
[0071] C. Polyamide purification: add 3% NaOH solution to the concentrated solution of step B to dissolve, mix the sample with polyamide 1:1, add 3% hydrochloric acid to adjust to neutrality, dry, perform polyamide column chromatography, ...
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