Steroid saponin compounds and preparation method and application thereof
A technology for steroidal saponins and compounds is applied in the field of steroidal saponins of Polygonatum japonica and their preparation fields, which can solve the problems of no reports on the content determination method, and achieve the effects of being convenient for industrialization and easy to operate.
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[0043] The preparation method of the compound is as follows: Polygonatum polygonatum is dried and pulverized at a temperature of -40°C to 60°C, and an aqueous solution of ethanol with a volume concentration of 50% to 70% is used as a mixed solvent, and the mass volume of Polygonatum polygonatum and the mixed solvent is mixed. The ratio is 1:2~20(g / mL) and mixed for ultrasonic extraction, 15℃~60℃ low temperature stirring extraction or reflux extraction; the extract is filtered and concentrated by ultrafiltration membrane and nanofiltration membrane equipment: in membrane concentration equipment The molecular weight cut-off of the membrane is 100-5000, concentrated to 1 / 10-1 / 2 of the volume of the extract; the concentrated solution is adsorbed by a macroporous resin column: macroporous resin column selection: AB-8, D101, D201, D301, HDP100, HDP400, XDA-1, XDA-5, XDA-6, XDA-8, LSA-20, LSA-30, LSA-40, HP-10, HP-20, HP-30, HP-40 or HP-50, Sequentially use water to remove impurities...
Embodiment 1
[0071] Structural formula (1) - purification and preparation of structural formula (8) compound
[0072] Polygonatum odoratum was dried and pulverized at a temperature of 30°C, weighed 150kg, and the aqueous solution of ethanol with a volume concentration of 70% was used as a mixed solvent, and extracted with low-temperature stirring at 30°C (3 times×1000L×2h), and the extract was passed through a membrane Concentration equipment for concentration: first pass ultrafiltration through a membrane system with a molecular weight cut-off of 3000, and then pass through the liquid through a membrane system with a molecular weight cut-off of 500 to obtain a concentrated solution of 200L; the concentrated solution is absorbed by a macroporous resin column HP-20, Sequentially use water, 30% ethanol aqueous solution elution to remove impurities, 70% ethanol aqueous solution elution, collect and combine the eluate; eluent adopts concentration equipment to recover ethanol, and spray-dries to...
Embodiment 2
[0074] Structural formula (1) - purification and preparation of structural formula (8) compound
[0075] Polygonatum odoratum was freeze-dried and pulverized at a temperature of -20°C, weighed 150kg, and used an aqueous solution of ethanol with a volume concentration of 70% as a mixed solvent for reflux extraction (3 times × 1500L × 2h), and the extract was passed through a membrane concentration equipment Concentration: First pass ultrafiltration through a membrane system with a molecular weight cut-off of 2500, and then pass through the liquid through a membrane system with a molecular weight cut-off of 600 to obtain a concentrated solution of 180L; the concentrated solution is absorbed by a macroporous resin column D101, followed by water, 35 After elution with an aqueous solution of ethanol to remove impurities, elution with an aqueous solution of 70% ethanol was carried out, and the combined eluent was collected; the eluent was reclaimed by a concentration device, and spra...
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