A kind of method for extracting flavonoids active ingredient in Chinese medicine Citrus aurantium
A technology of active ingredients and flavonoids, applied in the field of extraction and detection of natural medicines, to achieve high extraction efficiency and good extraction and detection results
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[0046] The specific steps of the preparation method of the Fructus Fructus reference substance solution are as follows: respectively take appropriate amounts of reference substances of neohesperidin and naringin, weigh them accurately, mix them in a brown measuring bottle, add methanol to make 500 μg of neohesperidin per 1 mL , A solution of 500 μg of naringin was obtained as a reference substance solution.
[0047] The ionic liquid bromide 1-ethyl-3-methylimidazole used in the embodiment of the present invention, 1-butyl-3-methylimidazole methanesulfonate, 1-hexyl-3-methylimidazole bromide, 1 -Butyl-3-methylimidazolium tetrafluoroborate and 1-hexylpyridine tetrafluoroborate were purchased from Alfa Aesar.
Embodiment 1
[0049] Weigh 150 mg of florisil and 50 mg of Fructus aurantii herb powder, add them into a mortar and grind for 1 min. Add the uniformly mixed solid mixture into five 3mL solid-phase extraction cartridges respectively, add a sieve plate to the bottom of the cartridge in advance, and then add a sieve plate to the top of the cartridge after the addition is complete. Place all filled cartridges on the solid phase extraction apparatus. Measure 0.4mL of different types of ionic liquid aqueous solutions, the ionic liquids are 1-ethyl-3-methylimidazole bromide, 1-butyl-3-methylimidazolium methanesulfonate, 1-hexyl-3-bromide -Methylimidazole, 1-butyl-3-methylimidazole tetrafluoroborate, 1-hexylpyridine tetrafluoroborate, the concentration of the above five ionic liquid aqueous solutions is 250mM, injected into the small column, start solidification The aspirating pump of the phase extractor (the air pressure is -28.0 bar) is used to elute the small column. The eluate was collected i...
Embodiment 2
[0057] Weigh 150 mg of florisil and 50 mg of Fructus aurantii herbal powder, and add them into a mortar and grind for 1 min. Add the well-mixed solid mixture to four 3mL SPE cartridges respectively, add a sieve plate to the bottom of the cartridge in advance, and then add a sieve plate to the top of the cartridge after the addition is complete. Place all filled cartridges on the solid phase extraction apparatus. Measure 0.4mL of 1-butyl-3-methylimidazolium tetrafluoroborate aqueous solution with different concentrations (150mM, 200mM, 250mM, 300mM), inject it into the small column, and start the aspirating pump of the solid phase extraction instrument (the air pressure is - 28.0bar), the column was eluted. The eluate was collected in 1.5mL centrifuge tubes respectively. After the elution, the liquid in the centrifuge tube was vortexed for 10s, then put into the centrifuge, and centrifuged at 13000rpm for 5min. The supernatant was collected as a sample, and analyzed by ultra...
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