Process for preparing tectori-genin
A technology of irisin and iris, which is applied in the field of preparation of irisin, can solve the problem of large-scale preparation of irisin, and achieve the effect of simple steps and high yield
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Embodiment 1
[0029] The dried iris rhizome is pulverized and taken 100 grams, added 3 times the amount (300ml) of 20% methanol solution, soaked for half an hour, then heated and refluxed in a water bath at 86°C for 6 hours, and filtered to obtain the filtrate after 6 hours. Repeat 3 times, combine the extracts obtained 3 times, and concentrate the filtrate to remove the solvent to obtain a paste. Add 400ml of 5% sodium bicarbonate solution to the paste to make the pH at 8.5, stir well and filter to obtain 400ml of clear filtrate. The alkaline solution was first extracted 3 times with 400 ml of chloroform, then extracted 3 times with 400 ml of ethyl acetate, and the combined ethyl acetate solution was concentrated and dried to obtain 1.8 g of yellow substance. The yellow substance was dissolved in 16 ml of methanol and recrystallized to obtain 1.4 g of irisinin with relatively high purity. After multiple recrystallizations, light yellow needle crystals are obtained, melting point 215-216°C...
Embodiment 2
[0033] The dried iris rhizome was pulverized and got 100 grams, added 15 times the amount (1500ml) of 90% methanol solution, soaked for half an hour, then heated and refluxed in a water bath at 86°C for 6 hours, and filtered to obtain the filtrate after 6 hours. The filtrate was concentrated to remove the solvent to obtain a paste. Add 400ml of 2% sodium bicarbonate solution to the paste to make the pH at 7.8, stir well and filter to obtain 400ml of clear filtrate. The alkaline solution was first extracted 4 times with 400 ml of chloroform, then extracted 4 times with 400 ml of ethyl acetate, and the combined ethyl acetate solution was concentrated and dried to obtain 1.9 g of a yellow substance. Dissolve the yellow substance with 38 ml of methanol, and recrystallize to obtain 1.2 grams of irisinin with higher purity, which is the same substance as irisinin in Example 1. The content of irisin is more than 80%. The content detection method of irisin (the same below):
[0034...
Embodiment 3
[0044] Grind the dried rhizome of iris and take 100 grams, add 3 times the amount (300ml) of water, soak and heat and reflux in a water bath at 100°C to extract for 6 hours, filter after 6 hours to obtain the filtrate and filter residue, and use 3 times the amount (300ml) of the filter residue again The water was extracted by heating and refluxing in a water bath at 100°C for 6 hours, and the two filtrates were combined and concentrated to obtain a paste. Add 400ml of 2% sodium carbonate to the paste, make the pH of the solution at 10.5, stir well and then filter to obtain a clear filtrate. Concentrated hydrochloric acid was added to the filtrate to make the filtrate acidic (pH 2.5), that is, substances were precipitated, and the precipitates obtained by filtration were total isoflavones (6.7 g in dry weight). Fully dissolve the above-mentioned total isoflavone precipitates with 400ml of 2% sodium bicarbonate solution, first extract the sodium bicarbonate solution 4 times with...
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