Method for preparing sodium aescinate
A technique for sodium aescinate and time control is applied in the preparation of sugar derivatives, chemical instruments and methods, steroids, etc., and can solve the problems of long production cycle, low yield of extracting sodium aescinate, low purity and the like, Achieve the effect of improving product yield, reducing environmental pollution and reducing impurity content
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Embodiment 1
[0018] (1) Extraction: The extraction temperature is 25°C, take 50kg of salsa seed powder and add 375L of 10% ethanol solution by volume to soak for 1 hour, extract for 2 hours, then filter to obtain the filter residue and filtrate respectively, and add the filter residue to 50L The ethanol solution with a volume percentage of 5% was extracted again for 2 hours and then filtered. The filtrates filtered twice should be clarified. The two filtrates should be combined, and the combined filtrates should be centrifuged with a plate centrifuge to collect the supernatant. The speed is 1000 rpm, and the centrifugation time is 1 hour;
[0019] (2) Chromatography: Put the washed D101 resin into the chromatography column to reach 4 / 5 column height, then add the extracted and centrifuged filtrate to the chromatography column for adsorption, the flow rate is 200 ml / min, use Acetic anhydride identification, stop adsorption when the effluent is nearly red; then wash the D101 resin with purif...
Embodiment 2
[0026] (1) Extraction: The extraction temperature is 37.5°C, take 50kg of salsa seed powder and add 150L of 10% ethanol solution by volume, soak for 1 hour, extract for 2 hours, and then filter to obtain the filter residue and filtrate respectively, and add the filter residue to 200L The ethanol solution with a volume percentage of 5% was extracted again for 2 hours and then filtered. The filtrates filtered twice should be clarified. The two filtrates should be combined, and the combined filtrates should be centrifuged with a plate centrifuge to collect the supernatant. The speed is 1300 rpm, and the centrifugation time is 1 hour;
[0027](2) Chromatography: Put the washed D201 resin into the chromatography column to reach 4 / 5 of the column height, then add the extracted and centrifuged filtrate to the chromatography column for adsorption, the flow rate is 300ml / min, and use vinegar Anhydride identification, stop adsorption when the effluent is nearly red; then wash the D201 r...
Embodiment 3
[0034] (1) Extraction: The extraction temperature is 40°C, take 50kg of salsa seed powder and add 600L of 10% ethanol solution by volume to soak for 1 hour, extract for 2 hours, then filter to obtain the filter residue and filtrate respectively, and add the filter residue to 125L The ethanol solution with a volume percentage of 5% was extracted again for 2 hours and then filtered. The filtrates filtered twice should be clarified. The two filtrates should be combined, and the combined filtrates should be centrifuged with a plate centrifuge to collect the supernatant. The speed is 1250 rpm, and the centrifugation time is 1 hour;
[0035] (2) Chromatography: put the washed NKA-9 resin into the chromatographic column to reach 4 / 5 column height, then add the extracted and centrifuged filtrate to the chromatographic column for adsorption, the flow rate is 250ml / min , identify with acetic anhydride, stop adsorption when the effluent is nearly red; then wash NKA-9 type resin with puri...
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