A new method for sulfation of fermented defatted rice bran
A degreased rice bran and sulfation technology is applied in the fields of biological, fermented defatted rice bran sulfation, and chemical modification of degreased rice bran. It can solve the problems of low yield, expensive reagents, and difficult reaction, achieve low boiling point, save manpower and material resources, and increase The effect of extraction rate
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Embodiment 1
[0036] Said 500g defatted rice bran semi-dry method to ferment. Add 15% purified water and 0.1% Bacillus subtilis, and ferment for 72 hours. dry.
[0037] Take 1000g of anhydrous acetonitrile in a dry bottle, cool to 0°C, add 2000g of fuming sulfuric acid dropwise under stirring, which is the sulfation reagent, and set aside.
[0038] Add 500g of acetonitrile to 50g of dry fermented rice bran, cool to 0°C, slowly add 1350g of sulfation reagent dropwise under stirring, after the dropwise addition, fully cool at 0°C, then stir and react in a 35°C water bath for 4 hours . After the reaction was completed, the flask was cooled at 0°C, stirred and added dropwise with 20% sodium hydroxide solution for neutralization until pH = 7, suction filtered, rotary evaporated, and lyophilized to obtain 46 g of the crude product.
[0039] Dialyze with MD55 dialysis bag deionized water for 2 days respectively, after concentration, pass through gel chromatography column (ultrafine Sephadex LH-...
Embodiment 2
[0044] Said 500g defatted rice bran semi-dry method to ferment. Add 15% purified water and 0.1% Bacillus subtilis, and ferment for 72 hours. dry.
[0045] Add 500g of acetonitrile to 50g of dry fermented rice bran, cool to 0°C, slowly add 1200g of sulfation reagent dropwise under stirring, after the dropwise addition, fully cool at 0°C, then stir and react in a 35°C water bath for 4 hours . After the reaction was completed, the flask was cooled at 0°C, stirred and added dropwise with 20% sodium hydroxide solution for neutralization until pH = 7, suction filtered, rotary evaporated, and freeze-dried to obtain 42 g of the crude product.
[0046]Dialyze with MD55 dialysis bag deionized water for 2 days respectively, after concentration, pass through gel chromatography column (ultrafine Sephadex LH-20, deionized water), mobile phase is deionized water, flow rate 0.4mL / min, TLC detects components ( Developing agent acetone: n-butanol: water = 1:1:1, developer: 10% sulfuric acid-...
Embodiment 3
[0048] Weighing 500g dry wheat bran semi-dry method is fermented. Add 15% purified water and 0.1% Bacillus subtilis, and ferment for 72 hours. dry.
[0049] Add 500g of acetonitrile to 50g of dry fermented wheat bran, cool to 0°C, slowly add 1350g of sulfation reagent dropwise under stirring, after the dropwise addition, fully cool at 0°C, then stir in a water bath at 35°C for reaction 4 Hour. After the reaction was completed, the flask was cooled at 0°C, stirred and added dropwise with 20% sodium hydroxide solution for neutralization until pH = 7, suction filtered, rotary evaporated, and freeze-dried to obtain 40 g of the crude product.
[0050] Dialyze with MD55 dialysis bag deionized water for 2 days respectively, after concentration, pass through gel chromatography column (ultrafine Sephadex LH-20, deionized water), mobile phase is deionized water, flow rate 0.4mL / min, TLC detects components ( Developing agent acetone: n-butanol: water = 1:1:1, developer: 10% sulfuric a...
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