Method for separating purifying ursolic acid from loquat leaf
A technology for separation and purification of ursolic acid, applied in medical preparations containing active ingredients, organic chemistry, pharmaceutical formulas, etc., can solve problems such as waste and unused applications, and achieve reduced preparation costs, improved dissolution rate, and low boiling point Effect
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Embodiment 1
[0035] Using loquat leaves produced in Putian, Fujian as raw materials, fresh loquat leaves are washed, dried (air-dried, dried or sun-dried), pulverized, and sieved with 20-30 meshes to obtain loquat leaf powder, and 2.6kg of loquat leaf powder is put into extraction. In the tank, use 85% methanol-acetone (1:1) aqueous solution of 12 times the dry weight (W / W) of loquat leaf powder to reflux and extract for 2 hours at 72°C, filter, and the filtrate is at -0.05~-0.09MPa. , under the condition of 50~70 ℃, the solvent is recovered under reduced pressure, vacuum concentrated into loquat leaf total triterpene acid extract; under 72 ℃ condition, the loquat leaf total triterpene acid extract uses 3 times the amount (W / W) of pH 90% methanol-acetone (1:1) aqueous solution (W / W) with a value of 10.9 was used to fully extract the total triterpene acid of loquat leaves, stand for aging, filter to remove insolubles, and add 1.3% (W / V) to the filtrate while it was still hot. Activated carb...
Embodiment 2
[0039] Put 2.8kg of loquat leaf powder degreased with petroleum ether of 20~30 meshes into the extraction tank, use 20 times the dry weight (W / W) of loquat leaf powder with a pH value of 3.2 70% methanol aqueous solution, under the condition of 50 ℃ Extracted twice, 3 hours each time, combined the extracts, filtered, the filtrate was recovered under reduced pressure under the conditions of -0.05~-0.09MPa and 50~70°C, and the solvent was recovered under reduced pressure, and concentrated in vacuo to obtain the loquat leaf total triterpene acid extract; 50 Under the condition of ℃, the total triterpene acid extract of loquat leaves was fully extracted with 15 times the amount (W / W) of 92% methanol aqueous solution (W / W) with a pH value of 8.0, and the total triterpenoid acids of loquat leaves were fully extracted, and then left to stand for aging and filtration. Remove insoluble matter, add 0.5% (W / V) activated carbon to the filtrate while hot for decolorization; add 50% sulfuric...
Embodiment 3
[0043] Put 2.9kg of 20-30 mesh loquat leaf powder that has undergone carbon dioxide supercritical extraction and deoiling treatment into the extraction tank, and use 5 times the dry weight (W / W) of the loquat leaf powder to extract at 80 °C. 2 hours, filter, under the conditions of -0.05~-0.09MPa and 50~70 ℃, the filtrate is recovered under reduced pressure, and the solvent is concentrated in vacuo to obtain the loquat leaf total triterpene acid extract; under the condition of 80 ℃, the loquat leaf total triterpene acid extract The extract was fully extracted with 10 times the amount (W / W) of 80% methanol aqueous solution (W / W) with a pH value of 8.9, and the total triterpene acid of loquat leaves was fully extracted. % (W / V) activated carbon for decolorization; the decolorized filtrate was added to a saturated aqueous citric acid solution while hot, and the final methanol concentration in the control system reached 25% (W / W) and the pH value was 5.5, and slowly cooled until th...
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