A kind of preparation method of aescin a
A escin and crystallization technology, applied in the preparation of sugar derivatives, chemical instruments and methods, steroids, etc., can solve the problems of patients prone to phlebitis, difficult industrial production, strong stimulation, etc., and achieve pharmacological activity Strong, less toxic, less environmental pollution effect
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Embodiment 1
[0025] 1) Extraction: take 1 kg of saffron seed powder and extract twice, each time with 10 L of ethanol aqueous solution with a mass concentration of 70%, stir and extract at 45°C for 2 hours, filter, combine the filtrates filtered twice, and rotate and recover under reduced pressure solvent and concentrated to 2L;
[0026] 2) Extraction: adjust the pH of the concentrated solution obtained in step 1) to 2 with 1 mol / L hydrochloric acid, extract 3 times with 2 L of water-saturated n-butanol, combine the organic layers and concentrate to 400 mL;
[0027] 3) The first crystallization: Add the concentrated solution obtained in step 2) into a mixed solvent of 960mL acetone and 240mL methyl tert-butyl ether, heat to reflux under stirring, then cool to 20°C to precipitate a white precipitate, filter, 45°C Dried to obtain 49g of white crystals;
[0028] 4) The second crystallization: Dissolve 49g of crystals obtained in step 3) in 200mL of hot water at 100°C, stir for 20min, then co...
Embodiment 2
[0037] 1) Extraction: take 1 kg of saffron powder and extract it under reflux three times, each time with 6L of 30% ethanol aqueous solution, filter, combine the filtrates, spin to recover the solvent under reduced pressure and concentrate to 2L;
[0038] 2) Extraction: adjust the pH of the concentrated solution obtained in step 1) to 3 with 3 mol / L hydrochloric acid, extract 3 times with n-butanol saturated with water, combine the organic layers and concentrate to 200 mL;
[0039] 3) The first crystallization: Add the concentrated solution obtained in step 2) into a mixed solvent of 300mL acetone and 100mL methyl tert-butyl ether, heat to reflux under stirring, then cool until a white precipitate precipitates, filter and dry to obtain a white crystal 38g;
[0040] 4) Second crystallization: Dissolve 38g of aescin crystals obtained in step 3) in 100ml of hot water at 80°C, stir for 60min, then cool the solution to precipitate a white solid, filter it with suction, and dry the ...
Embodiment 3
[0045] 1) Extraction: take 1 kg of the saffron seed powder and reflux for extraction twice, each time with 15 L of ethanol solution with a mass concentration of 50%, filter, combine the filtrates, spin to recover the solvent under reduced pressure and concentrate to 3 L;
[0046] 2) Extraction: adjust the pH of the concentrated solution obtained in step 1) to 3 with 0.5 mol / L hydrochloric acid, extract 5 times with n-butanol saturated with water, combine the organic layers and concentrate to 300 mL;
[0047] 3) The first crystallization: Add the concentrated solution obtained in step 2) into a mixed solvent of 1200mL acetone and 150mL methyl tert-butyl ether, heat to reflux under stirring, then cool until a white precipitate precipitates, filter and dry to obtain a white crystal 43g;
[0048] 4) Second crystallization: Dissolve 43g of aescin crystals obtained in step 3) in 215mL of boiling water, stir for 30min, then cool the solution to precipitate a white solid, centrifuge, ...
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