Method for separating genistein from isoflavone genin mixture
A technology of isoflavone aglycone and genistein, which is applied in the field of separation of genistein and genistein from soybean isoflavone aglycone mixture, and can solve the problem of difficult to have the selective extraction ability of soybean isoflavone aglycon homologues, etc. problems, achieve high selective separation ability, reduce pollution, facilitate recycling and utilization
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Embodiment 1
[0043] The commercially available soybean isoflavone crude product (produced by Heilongjiang Jiusan Oil Co., Ltd.), which contains 40% mass fraction of soybean isoflavone glucoside, was recrystallized 4 times with 75% ethanol aqueous solution, washed with water and suction filtered , to obtain a crude product containing soybean isoflavone glycosides after vacuum drying. The obtained crude product containing soybean isoflavone glycosides is hydrolyzed with 1mol / L sulfuric acid as a catalyst, and 75% ethanol aqueous solution as a solvent, and the hydrolysis reaction product solution is filtered to obtain a solid containing soybean isoflavone aglycones The mixture is washed with water until neutral, recrystallized four times with n-butanol, and vacuum-dried to obtain the raw material soybean isoflavone aglycone mixture.
[0044] The raw material soybean isoflavone aglycon mixture (wherein the total weight percent content of daidzein, genistein and glycitein is 95%) and n-propanol...
Embodiment 2
[0046] The preparation of the raw material soybean isoflavone aglycone mixture is the same as that in Example 1, except that the solvent for the recrystallization of soybean isoflavone aglycone is 75% ethanol aqueous solution.
[0047] The raw material soybean isoflavone aglycone mixture (wherein the total weight percent content of daidzein, genistein and glycitein is 90%) and n-amyl alcohol is formulated into the total amount of daidzein, genistein and glycitein Raw material solution with a concentration of 0.5 g / L. With 1-butyl-3-methylimidazolium chloride ([bmim]Cl)-water mixed solvent as extractant ([bmim]Cl molar fraction 65%), with n-amyl alcohol as detergent, extractant, detergent, The flow ratio of the three raw materials is 4:3:2, fractionation extraction is carried out in a fractionation extraction device at 20° C., the extract is collected, and genistein is obtained after n-pentanol back extraction and vacuum concentration. HPLC analysis showed that the purity of g...
Embodiment 3
[0049] The preparation of the raw material soybean isoflavone aglycone mixture, except that the number of recrystallization of soybean isoflavone glucoside is 3 times, and the recrystallization solvent of soybean isoflavone aglycone is an ethanol aqueous solution with a concentration of 75% by volume, the rest of the operations are carried out in the same way example 1.
[0050] Raw material soybean isoflavone aglycone mixture (wherein the total weight percent content of daidzein, genistein and glycitein is 60%) and water is made into the total concentration of daidzein, genistein and glycitein as 0.6 g / L of raw material solution. With 1-hexyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide salt ([hmim][NTf 2 ]) is the extraction agent, water is the detergent, the flow ratio of the extraction agent, the detergent, and the raw material liquid is 3: 2: 1.5, and fractionation extraction is carried out in a fractionation extraction device at 60° C., the extract is collecte...
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