Method for extracting robinin from robinia pseudoacacia flowers
A technology of locust glycoside and locust flower, which is applied in the field of ultrasonic-microwave collaborative extraction of locust glucoside, which can solve the problems of difficult large-scale production, large amount of ethanol, and high equipment cost, and achieve low solvent toxicity, stable product quality, and low preparation cost. Effect
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Embodiment 1
[0015] Take Robinia pseudoacacia flowers, remove impurities, dry at 60°C, crush, pass through a 80-mesh sieve, take 1kg of powder and add 9 times the 60% ethanol solution, soak for 30 minutes, use ultrasonic-microwave to extract, control ultrasonic 400W (normally open ), with a microwave power of 500W, extract for 2 hours, centrifuge, take the supernatant, concentrate, dissolve the concentrate in water, and absorb it through a neutral alumina column. The particle size of the neutral alumina is 50 mesh. The mass ratio of alumina is 1:4, the height-to-diameter ratio of the column is 4:1, 10 times of 50% ethanol is used for elution, the eluate is collected, concentrated under reduced pressure, and the crude acaciaside is obtained, and then ethanol-methanol ( 1:1) mixed solvent recrystallization twice to obtain 20.8 g of acaciaside, which was detected by HPLC with a purity of 97.9%.
Embodiment 2
[0017] Take Robinia pseudoacacia flowers, remove impurities, dry at 60°C, crush, pass through a 80-mesh sieve, take 1kg of powder and add 6 times the 65% ethanol solution, soak for 50min, use ultrasonic-microwave to extract, control ultrasonic 400W (normally open ), the microwave power is 550W, extract for 2.5h, centrifuge, take the supernatant, concentrate, the concentrate is heated to dissolve in water, and adsorbed by a neutral alumina column. The particle size of the neutral alumina is 80 mesh. The mass ratio of permanent alumina is 1:5, the height-diameter ratio of the column is 7:1, 12 times of 60% ethanol is used for elution, the eluate is collected, and concentrated under reduced pressure to obtain the crude acaciaside, which is then ethanol-methanol (1:1) mixed solvent was recrystallized twice to obtain 23.1 g of acaciaside, which was detected by HPLC with a purity of 98.7%.
Embodiment 3
[0019] Take Robinia pseudoacacia flowers, remove impurities, dry at 60°C, crush, pass through a 80-mesh sieve, take 1kg of powder and add 4 times the 70% ethanol solution, soak for 60 minutes, use ultrasonic-microwave to extract, control ultrasonic 400W (normally open ), with a microwave power of 600W, extract for 3 hours, centrifuge, take the supernatant, concentrate, dissolve the concentrate in heated water, and pass through a neutral alumina column for adsorption. The mass ratio of alumina is 1:6, the height-to-diameter ratio of the column is 10:1, 15 times of 70% ethanol is used for elution, the eluate is collected, concentrated under reduced pressure to obtain the crude acaciaside, and then ethanol-methanol ( 1:1) mixed solvent recrystallization twice to obtain 21.4 g of acaciaside, which was detected by HPLC with a purity of 98.4%.
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