A kind of preparation method of jujube seed saponin A reference substance
A technology of jujube seed saponin and reference substance, which is applied in the fields of steroids and organic chemistry, and can solve problems such as difficulty in separating monomers, low content of jujube seed saponin A, and insufficient supply
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[0049] Preparation method of the present invention
[0050] For realizing above-mentioned purpose of the invention, the technical scheme that the present invention adopts is as follows:
[0051] A kind of preferred technical scheme of the present invention is as follows:
[0052] A. Extraction of raw materials: adding 5 to 8 times the amount of ethanol solution according to the volume and mass ratio L / Kg of the Chinese date seed medicinal material, and the volume percentage concentration of the used ethanol solution is 60-75%; Heat extraction at least 2 times at ℃, about 2 hours each time, cool to room temperature, filter with suction, combine the filtrates, and concentrate until there is no alcohol smell;
[0053] B. macroporous resin enrichment: the concentrated solution of step A is statically adsorbed overnight with macroporous resin, and then use 2-3 times of column volume water and 2-5 times column volume of 15-30% ethanol solution Elute the impurities, and then use 1-...
Embodiment 1
[0066] The preparation method of jujuboside A reference substance, it is carried out according to the following process steps:
[0067] A. Raw material extraction: Add 100Kg of jujube seed medicinal material to 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;
[0068] B. Enrichment of macroporous resin: Weigh 20KgD101 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 80L of water and 30% ethanol solution of 50L column volume respectively Elute the impurities, then elute the target substance with 30L of 60% ethanol solution, collect the eluate, and concentrate to 1000ml;
[0069] C. Extraction: Add 2000ml of n-butanol to the concentrated solution of step B, extract, collect th...
Embodiment 2
[0079] A. Raw material extraction: Add 500Kg of Chinese jujube seed medicinal material to 2500L of 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, 150L in total;
[0080] B. Macroporous resin enrichment: Weigh 100KgD101 macroporous adsorption resin and pack it into a column, statically adsorb the concentrated solution of step A with macroporous resin for 20 hours overnight, and then use 400L of water and 30% ethanol solution of 250L column volume respectively Elute the impurities, then elute the target substance with 150L of 60% ethanol solution, collect the eluate, and concentrate to 5000ml;
[0081] C. Extraction: Add 10L n-butanol to the concentrated solution of step B, extract, collect the n-butanol layer, and concentrate to obtain the ethanol extract of jujuboside A described in step (i);
[0082] D. Mediu...
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