Method for preparing sesamin from sesame
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Embodiment 1
[0032] Get 20kg of sesame seeds (0.4% of sesamin content), pulverize, add 80L 95% edible ethanol, reflux extraction for 2 hours, extract 3 times, combine extracts, recover ethanol by vacuum distillation, concentrate into extract, wash with 10% ammonia water, Centrifuge to obtain 1.2kg of extract, dissolve it in chloroform, filter, add 7kg of 80-100 mesh neutral alumina, stir and mix, and recover chloroform. Take 7L of D101 macroporous resin, pack it into a column, add a 200-mesh screen to the upper part, then mix the sesamin sample into it, first elute the fat-soluble impurities with 56L of 6# solvent oil, and then use ethyl acetate methanol 1:1 (v / v) The mixed solution elutes low-polarity impurities. TLC detects that sesamin flows out, and then elutes with ethyl acetate methanol 1:10 (v / v) until there is no sesamin fraction. Collect this fraction, recover the reagent to 1 / 6 of its volume and place it for crystallization, grow the crystal for 4 hours, and filter out 102 g of ...
Embodiment 2
[0034] Get 20kg of sesame seeds (0.4% of sesamin content), pulverize, add 120L 90% edible ethanol, reflux extraction for 2 hours, extract twice, combine extracts, recover ethanol by vacuum distillation, concentrate into extract, wash with 8% ammonia water, Centrifuge to obtain 1 kg of extract, then dissolve in chloroform, filter, add 6 kg of 80-100 mesh neutral alumina, stir and mix, and recover chloroform. Take 6L of macroporous resin, pack it into a column, add a 200-mesh screen to the upper part, then mix the sesamin sample into it, first elute fat-soluble impurities with 48L of 6# solvent oil, and then use ethyl acetate methanol 1:1 (v / v) The mixed solution elutes low-polarity impurities. TLC detection shows that sesamin flows out. Use ethyl acetate methanol 1:10 (v / v) for elution until there is no sesamin fraction. Collect this fraction, recover the reagent to 1 / 10 of its volume and place it for crystallization, grow the crystal for 6 hours, and filter out 96 g of crude c...
Embodiment 3
[0036] Get 20kg of sesame seeds (0.4% of sesamin content), pulverize, add 100L 85% edible ethanol, reflux extraction for 2 hours, extract 3 times, combine extracts, recover ethanol by vacuum distillation, concentrate into extract, wash with 10% ammonia water, Centrifuge to obtain 1.1 kg of extract, then dissolve in chloroform, filter, add 5 kg of 80-100 mesh neutral alumina, stir and mix, and recover chloroform. Take 7 liters of macroporous resin, pack it into a column, add a 200-mesh screen to the upper part, then mix the sesamin sample into it, first elute the fat-soluble impurities with 6# solvent oil 60L, and then use ethyl acetate methanol 1:1 (v / v ) mixed solution to elute low-polarity impurities, TLC detection, sesamin flow out, use ethyl acetate methanol 1:10 (v / v) to elute until there is no sesamin fraction. Collect this fraction, recover the reagent to 1 / 10 of its volume and place it for crystallization, grow the crystal for 6 hours, and filter out 102 g of the crude...
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Abstract
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