Method for extracting and separating agapanthussaponin A
A separation method and saponin technology, which is applied in the field of extraction and separation of saponin Ⅲ, can solve problems such as saponin Ⅲ that have not been seen yet, and achieve the effect of reducing sample loss, large amount of preparation, and good separation effect
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Embodiment 1
[0018] The underground part of the broad-leaved soil Ophiopogon japonicus is crushed, weighed 3kg, and added to a supercritical extraction kettle for supercritical CO extraction. 2 Extraction, extraction temperature is 60°C, extraction pressure is 25MPa, analysis temperature is 50°C, analysis pressure is 9MPa, CO 2 The flow rate is 20L / h, remove oily substances, release raw material residues, add 80% ethanol solution for microwave extraction 3 times, microwave extraction power is 800w, filter to obtain extract, concentrate to extract, add appropriate amount of water to disperse, add 3 Extract twice the amount of water-saturated n-butanol twice, add 0.5 times the amount of acetone to the combined extracts, filter, concentrate and dry the filtrate to obtain the crude product; use petroleum ether-ethyl acetate-ethanol-water (8:4:7:6) As a two-phase solvent system, after mixing, put it in a separatory funnel and let it stand for stratification. Take the upper phase as the stationa...
Embodiment 2
[0020] The underground part of the broad-leaved soil Ophiopogon japonicus is crushed, weighed 3kg, and added to a supercritical extraction kettle for supercritical CO extraction. 2 Extraction, extraction temperature is 40°C, extraction pressure is 15MPa, analysis temperature is 30°C, analysis pressure is 5MPa, CO 2 The flow rate is 18L / h, remove oily substances, release raw material residues, add 70% ethanol solution for microwave extraction 3 times, microwave extraction power is 600w, filter to obtain extract, concentrate to extract, add appropriate amount of water to disperse, add 1 Extract three times the amount of water-saturated n-butanol, combine the extracts and add 1 times the amount of acetone to precipitate, filter, concentrate and dry the filtrate to obtain the crude product; use petroleum ether-ethyl acetate-ethanol-water (6:4:7:6) As a two-phase solvent system, after mixing, put it in a separatory funnel and let it stand for stratification. Take the upper phase as...
Embodiment 3
[0022] The underground part of the broad-leaved soil Ophiopogon japonicus is crushed, weighed 3kg, and added to a supercritical extraction kettle for supercritical CO extraction. 2 extraction, extraction temperature is 50°C, extraction pressure is 20MPa, analysis temperature is 40°C, analysis pressure is 7MPa, CO 2 The flow rate is 20L / h, remove oily substances, release raw material residues, add 70% ethanol solution for microwave extraction twice, microwave extraction power is 800w, filter to obtain extract, concentrate to extract, add appropriate amount of water to disperse, add 2 Double the amount of water-saturated n-butanol and extract twice, combine the extracts and add 0.8 times the amount of acetone to precipitate, filter, concentrate and dry the filtrate to obtain the crude product; use petroleum ether-ethyl acetate-ethanol-water (7:3:6:5) As a two-phase solvent system, after mixing, put it in a separatory funnel and let it stand for stratification. Take the upper pha...
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