Process for producing ursolic acid
A technology of ursolic acid, precipitation and crystallization, which is applied in the direction of medical preparations containing active ingredients, pharmaceutical formulas, steroids, etc., can solve the problems of high cost, low product yield, complicated process, etc., and achieve low cost and high product quality. The effect of high yield and simple process
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Embodiment 1
[0020] Take chicle leaves (Alstonia scholaris) as a raw material, extract 1 kg of crushed chicle leaves with 1:3 times V / V industrial ethanol for 3 times, heat and reflux for 2 hours each time, combine the extracts, and recover the solvent to obtain chicle leaves Extract 230g. Add 0.2% hydrochloric acid aqueous solution to dissolve in extractum, fully stir, separate acid aqueous solution and precipitation, share 0.2% hydrochloric acid aqueous solution soak 4 times, merge acid aqueous layer, precipitation is ursolic acid crude product 96g. Add 2L of ethanol to the obtained precipitate to dissolve, and the solution is placed in a low temperature of 0°C for precipitation and crystallization. Once crystallized, 81g of ursolic acid can be obtained, and after multiple recrystallizations, ursolic acid with a purity of 98% can be obtained.
[0021] The obtained ursolic acid finished product is tested instrument, condition and result:
[0022] Instruments: Waters Alliance 2695 high pe...
Embodiment 2
[0026] Take sugar gum leaves (Alstonia scholaris) as raw material, extract 1 kg of crushed sugar gum leaves with 1:4 times (V / V) industrial ethanol reflux for 4 times, heat and reflux for 1.5 hours each time, combine the extracts, recover the solvent to obtain sugar Gum leaf extract 228g. Add 2L of 2% sulfuric acid aqueous solution to the extract to dissolve, fully stir, soak the extract for 4 times in 2% sulfuric acid aqueous solution, and separate the acid aqueous solution and the precipitate. The precipitate was 90 g of crude ursolic acid. Add 2L of ethanol in the precipitation to dissolve, and the solution is placed at 5°C for precipitation and crystallization. Through HPLC content detection, 78g of 41% ursolic acid can be obtained in one crystallization, and 98% ursolic acid with a purity of 98% can be obtained after multiple recrystallizations.
Embodiment 3
[0028] Take sugar gum leaves (Alstonia scholaris) as a raw material, boil 1 kg of crushed sugar gum leaves in water for 3 times, each time for 1 hour, remove water-soluble impurities, and use 1:10 times (V / V) industrial The ethanol was refluxed for 3 times, heated and refluxed for 1 hour each time, the extracts were combined, and the solvent was recovered to obtain 220 g of sugar gum leaf extract. Add 2L of 2% hydrochloric acid aqueous solution to the extract for dissolving, fully stir, soak the extract for 4 times in 2% hydrochloric acid aqueous solution, and separate the acid aqueous solution and the precipitate. The precipitate was 88g of crude ursolic acid. Add 2L of ethanol to the precipitate to dissolve, and place the solution at 5°C for precipitation and crystallization. After content detection by HPLC, 52g of crude ursolic acid can be obtained in one crystallization, and ursolic acid with a purity of >98% can be obtained through multiple recrystallizations.
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