Method for preparing arctiin
A technology of arctiin and arctium, which is applied in the field of natural medicine preparation, can solve the problems of long separation process, difficult recycling of solvent system, and low degree of separation automation, so as to reduce energy consumption, facilitate automatic production, facilitate recycling and The effect of recycling
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Embodiment 1
[0022] After crushing 50 g of Arctium Fructus into a 60-mesh coarse powder, add 10 times the amount of water to reflux for extraction twice for 2 hours, and combine the filtrates.
[0023] The obtained extract was directly entered into the HP-20 macroporous adsorption resin adsorption column for adsorption and enrichment, and then successively eluted with four gradients of water and mass concentrations of 30%, 60%, and 95% ethanol, and the eluent was washed with High performance liquid chromatography (HPLC) for analysis. HPLC detection column model: Zorbax SB-C18, 250mm×4.6mm I.D., 5μm and pre-column model: 10mm×4.6mm I.D., 5μm. The analysis conditions are: the mobile phase is (A) methanol, and (B) the mass fraction is 0.5% acetic acid. Gradient elution is within 0-25 minutes, the volume fraction of mobile phase (A) is from 30% to 90%; the volume fraction of mobile phase (B) is from 70% to 10%. Flow rate: 0.8 ml / min; UV absorption wavelength: 280nm; column temperature: 30°C....
Embodiment 2
[0027] After crushing 50 g of burdock fruit into a 60-mesh coarse powder, add 15 times the amount of water to reflux for extraction twice for 2 hours, and combine the filtrates.
[0028] The obtained extract was directly entered into the HP-20 macroporous adsorption resin adsorption column for adsorption and enrichment, and then successively eluted with four gradients of water and mass concentrations of 30%, 60%, and 95% methanol, and the eluent was washed with Analysis by HPLC. HPLC detection column model: Zorbax SB-C18, 250mm×4.6mm I.D., 5μm and pre-column model: 10mm×4.6mm I.D., 5μm. The analysis conditions are: the mobile phase is (A) methanol, and (B) the mass fraction is 0.5% acetic acid. Gradient elution is within 0-25 minutes, the volume fraction of mobile phase (A) is from 30% to 90%; the volume fraction of mobile phase (B) is from 70% to 10%. Flow rate: 0.8 ml / min; UV absorption wavelength: 280nm; column temperature: 30°C. The 60% methanol eluate containing arctii...
Embodiment 3
[0032] After crushing 50 g of Arctium Fructus into a 60-mesh coarse powder, add 10 times the amount of water to reflux for extraction twice for 2 hours, and combine the filtrates.
[0033] Put the obtained extract directly into the HP-20 macroporous adsorption resin adsorption column for adsorption and enrichment, first elute with water and 30% ethanol, then use water-saturated ethyl acetate eluent, switch the six-way valve, and water-saturated The ethyl acetate eluent was switched to the sample loop in countercurrent chromatography.
[0034] The resulting 60% ethanol eluate containing arctiin was separated by countercurrent chromatography using a two-phase system of ethyl acetate-5% aqueous solution of sodium chloride as a solvent system, with ethyl acetate as the upper phase and 6% chlorine An aqueous solution of sodium chloride was the lower phase.
[0035]Turn on the countercurrent chromatography (900 rpm, column volume 270mL), inject the sample, switch to the macroporous...
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