Method for preparing salvianolic acid B through separation by means of flash chromatography
A chromatographic separation and salvianolic acid technology, applied in organic chemistry and other directions, can solve the problems of difficult production and storage of traditional Chinese medicine preparations, high requirements for equipment and reagents, and difficulty in large-scale production. Degradation reduction effect
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Embodiment 1
[0039] 1. Medicinal material processing
[0040] Take Danshen decoction pieces, crush them, take 15g and add 50% ethanol by volume fraction at a ratio of 1:20 (m / v), soak for 6 hours, sonicate for 1 hour, filter, and add 50% ethanol by volume fraction at a ratio of 1:20 (m / v) to the residue Extract again for 1h and filter. Combine the filtrates extracted twice, concentrate under reduced pressure to 1 / 4 of the original volume, filter, and extract the filtrate 3 times with diethyl ether volume ratio (1:1), add 1mol L -1 Adjust the pH to 3 with HCl, filter, and extract the filtrate 3 times with ethyl acetate in a volume ratio (1:1), combine the ethyl acetate layers, and concentrate to dryness under reduced pressure to obtain ethyl acetate extract (0.65 g).
[0041] 2. Sample Processing
[0042] Take 100mg of ethyl acetate extract, add 25% volume fraction of methanol water and dissolve it to prepare a concentration of 30mg·mL -1 The solution was centrifuged for 10min (15000rpm)...
Embodiment 2
[0057] 1. Medicinal material processing
[0058] Take Danshen decoction pieces, crush them, take 15g, add 50% ethanol by volume fraction at a ratio of 1:20 (m / v), soak for 6 hours, ultrasonicate for 1 hour, filter, and add 50% ethanol by volume fraction at a solid-liquid ratio of 1:20 to extract again ,filter. Combine the filtrates extracted twice, concentrate under reduced pressure to 1 / 4 of the original volume, filter, and extract the filtrate 3 times with diethyl ether volume ratio (1:1), add 1mol L -1 HCl was adjusted to pH = 4, filtered, and the filtrate was extracted three times with ethyl acetate in a volume ratio (1:1). The ethyl acetate layers were combined and concentrated to dryness under reduced pressure to obtain ethyl acetate extract (0.62 g).
[0059] 2. Sample Processing
[0060] Take 120mg of ethyl acetate extract, add 25% volume fraction of methanol water and dissolve it to prepare a concentration of 60mg·mL -1 The solution was centrifuged for 10min (15000...
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