Method for extracting haw leaf general flavone material for injection using polyamide column
A technology of hawthorn leaves and total flavonoids is applied in the directions of plant raw materials, pharmaceutical formulations, medical preparations containing active ingredients, etc. Residue reduction and protection of natural properties
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Embodiment 1
[0012] Take dried hawthorn leaves, soak them with 10 times the amount of crude drug for three times at 60°C for 2 hours each time, combine the extracts, filter, and concentrate the filtrate under reduced pressure to contain crude drug 0.5g / ml, and add ethanol until the alcohol content reaches 60 %, let stand and refrigerate for 12 hours. Aspirate the supernatant, concentrate under reduced pressure until it has no alcohol taste, add deionized water to 0.2-0.5g / ml of crude drug, let stand, refrigerate for 12 hours, filter, and filter the filtrate on a polyamide chromatography column and wash with deionized water to The α-naphthol concentrated sulfuric acid reaction is negative, the water washing solution is discarded, and then 30% ethanol is used to elute until there is no hydrochloric acid-magnesium powder reaction. The ethanol eluate was collected, concentrated under reduced pressure to a thick paste, and dried under reduced pressure in a vacuum drying cabinet at 60° C. to a powde...
Embodiment 2
[0014] Take the dried hawthorn leaves and warm them with 15 times the amount of crude drug for three times at 70°C for 1.5 hours each time. Combine the infusions and filter. The filtrate is concentrated under reduced pressure to 0.7g / ml crude drug, and ethanol is added until the alcohol content reaches 70. %, let stand and refrigerate for 24 hours. Aspirate the supernatant, concentrate under reduced pressure until it has no alcohol taste, add deionized water to 0.3g / ml of crude drug, let stand, refrigerate for 24 hours, filter, and filter the filtrate on a polyamide chromatography column and wash with deionized water to α- The reaction of naphthol concentrated sulfuric acid is negative, the water washing solution is discarded, and then 30% ethanol is used to elute until the reaction of hydrochloric acid-magnesium powder is free. The ethanol eluate was collected, concentrated under reduced pressure to a thick paste, and dried under reduced pressure in a vacuum drying cabinet at 60°...
Embodiment 3
[0016] Take 10 kg of dried hawthorn leaves and soak them with 17 times the amount of crude drug at 90°C for three times for 2 hours each time. Combine the infusions and filter. The filtrate is concentrated under reduced pressure to 1.5g / ml crude drug, and ethanol is added until the alcohol content reaches 90%, let stand and refrigerate for 24 hours. Aspirate the supernatant and concentrate under reduced pressure until there is no alcohol, add deionized water to 40L of crude drug, let stand, refrigerate for 24 hours, filter, and filter the filtrate on a polyamide chromatography column, wash with deionized water to a concentration of α-naphthol The sulfuric acid reaction is negative, discard the washing liquid, and then eluted with 50% ethanol until the hydrochloric acid-magnesium powder reaction stops. The ethanol eluate was collected, concentrated under reduced pressure to a thick paste, and dried under reduced pressure in a vacuum drying cabinet at 60° C. to a powder, to obtain 1...
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