Method for effective preparation of salvianolic acid B extract
A technology of salvianolic acid and extract, which is applied in the field of extraction and separation and purification of natural products, can solve the problems of large amount of extracted impurities, excessive degradation of salvianolic acid B, and low purity of the extract, and achieve high physiological activity and salvianolic acid The effect of high acid B content
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Embodiment 1
[0050] (1) Take the Danshen medicinal residues extracted with 80% ethanol solution, add pH 5, and extract twice with 50% ethanol solution (the amount of solvent is 5 times the amount of dry medicinal residues / time, and the extraction time is 1.5 hours / time), extract liquid filtration, combined, and discarded medicinal residues;
[0051] (2) The specific gravity of the extract below 60°C is 0.95 (56°C) to obtain a concentrate; the concentrate is cooled to below 20°C to obtain a cooled concentrate;
[0052] (3) Stir the cooled concentrated solution and add 10% hydrochloric acid solution to adjust the pH value to 1.96, carry out acid precipitation, refrigerate below 10°C for 13 hours, and filter the pulp plate frame to obtain the filtrate;
[0053] (4) The filtrate is separated and purified by column chromatography: ①The filler is AB-8 resin, and the dosage is the ratio of resin swelling volume (ml) to medicinal material weight (g) 1:1; ②The flow rate of the sample is 1BV-3BV res...
Embodiment 2
[0056] (1) Take the dried rhizome of Salvia miltiorrhiza and extract the wet medicine dregs with 85% ethanol, and add the ethanol solution with a pH value of 2 and an alcohol content of 30% to extract once (the amount of solvent is 2 times (v / w) dry medicine amount of dregs, the extraction time is 0.5 hours), the extract is filtered, and the dregs are discarded;
[0057] (2) Concentrate the extract at 40°C to a specific gravity of 0.8 (56°C) to obtain a concentrated solution; cool down to 0°C to obtain a cooled concentrate;
[0058] (3) Stir the cooled concentrated solution and add 10% (v / v) sulfuric acid solution to adjust the pH value to 1, carry out acid precipitation, leave the concentrated solution at 2°C for 1 hour, and filter the pulp plate frame to obtain the filtrate;
[0059] (4) The filtrate is separated and purified by column chromatography: ①The filler is D101 resin, and the dosage is the ratio of resin swelling volume to the amount of medicinal material 0.5:1 (v / ...
Embodiment 3
[0062] (1) Take the wet dregs of fresh salvia miltiorrhiza after being extracted with 90% ethanol solution, add PH value to 8, and extract 5 times with ethanol solution with 60% alcohol content (the amount of solvent is 15 times (v / w) dry The amount of dregs / time, the extraction time is 5 hours / time), the extract is filtered and combined, and the dregs are discarded;
[0063] (2) Concentrate the extract at 100°C to a specific gravity of 1.20 (56°C) to obtain a concentrated solution; cool down to 25°C and place it for 24 hours to obtain a cooled concentrate;
[0064] (3) Stir the cooled concentrated solution and add 10% (v / v) acetic acid solution to adjust the pH value to 3, carry out acid precipitation, leave the concentrated solution at 20°C for 48 hours, and filter the pulp plate frame to obtain the filtrate;
[0065] (4) The filtrate is separated and purified by column chromatography: ①The filler is polyamide resin, and the dosage is the ratio of resin swelling volume to th...
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