Method for separating high-purity anthocyanin monomers from black rice
Anthocyanin, high-purity technology, applied in the direction of preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of restricting the development and utilization of anthocyanins, small output, and many impurities, so as to be suitable for large-scale production, Large sample loading and good selectivity
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Embodiment 1
[0019] Implementation Example 1: Take 5kg of black rice, grind 300g of rice skin, mix with 3L of 60% ethanol (containing 0.1% HCl), extract 2 times at room temperature, each 4-6h; Filtrate, and the filtrate was rotary evaporated at = 42°C until there was no ethanol; degreased with petroleum ether, filtered and passed through a pre-acidified macroporous resin adsorption column at a flow rate of 1-1.5 column volume / h, and washed off with 0.01% HCl after the adsorption was completed Impurities; elute with 80% ethanol solution, the flow rate is 2-3 column volumes / h, collect the eluent and rotate evaporate at 45°C until there is no ethanol to obtain anthocyanin extraction concentrate; connect three 40g medium-pressure chromatographic columns in series, inject Sample loading, 0.1% trifluoroacetic acid aqueous solution (A) and methanol (B) were used as mobile phase gradient elution, and the absorption peaks with corresponding retention times were collected to obtain 228mg Cy-3-G and 3...
Embodiment 2
[0020] Implementation Example 2: Take 25kg of black rice, grind 1500g of rice skin, mix with 15L of 60% ethanol (containing 0.1% HCl), extract 2 times at room temperature, each 4-6h; Filtrate, and the filtrate was rotary evaporated at = 42°C until there was no ethanol; degreased with petroleum ether, filtered and passed through a pre-acidified macroporous resin adsorption column at a flow rate of 1-1.5 column volume / h, and washed off with 0.01% HCl after the adsorption was completed Impurities; elute with 80% ethanol solution, the flow rate is 2-3 column volumes / h, collect the eluent and rotate evaporate at 45°C until there is no ethanol to obtain anthocyanin extraction concentrate; use a guard column (about 12g C18 packing) and glass The separation column (400g C18 filler, 50mm×500mm) was loaded with samples, 0.1% trifluoroacetic acid aqueous solution (A) and methanol (B) were used as mobile phase gradient elution, and the corresponding retention time absorption peaks were col...
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