Technique for extracting and separating salidroside from glossy privet fruit
A technology for salidroside and salidroside crude products, which is applied in the field of extraction and separation technology of salidroside in Ligustrum lucidum, a plant of Oleaceae, can solve the problem of low content of salidroside crude products, and achieve easy follow-up processing , content increase, low toxicity effect
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[0041] (b) Preparation of reference substance solution: Accurately weigh 1.1 mg of salidroside standard substance to obtain 1.1 mg / mL salidroside standard substance solution; accurately weigh 2.25 mg of tyrosol standard substance to obtain 225 μg / mL tyrosol standard solution. Then accurately draw 0.3 mL and 0.1 mL of the above two standard solutions in turn to make a mixed solution of the two standards, in which the concentration of the standard salidroside is 330 μg / mL, and the concentration of the standard tyrosol is 22.5 μg / mL .
[0042] (c) Preparation of the test solution: Weigh the dry extract of Ligustrum lucidum water extract (or the dry extract after hydrolysis), add 20% methanol to dissolve, set the volume in a 10 mL volumetric flask, and pass through a 0.45 μm micro Pore filter membrane, take the continued filtrate, that is.
[0043] (d) Determination method: Precisely draw and mix 10 μL of the reference substance solution and 20 μL of the test solution, inject it...
Embodiment 1
[0051] Take the dried and mature fruit of Ligustrum lucidum of the genus Ligustrum in the family Oleaceae, crush it to a coarse powder, add 8 times the amount of water to reflux and extract 3 times, each time is 2 hours, combine the extracts, and recover the solvent under reduced pressure at 80 ° C to obtain dried Extract concentration of 0.05 g / mL is Ligustrum lucidum concentrate, of which the yield of dry extract is 25.1%, and the content of salidroside is 1.65%. The dry extract concentration of 0.05 g / mL means that 1 mL of concentrated solution contains 0.05 g of dry extract, that is, 0.5 mg of dry extract can be obtained by recovering the solvent from 1 mL of concentrated solution to dryness.
[0052] Take 2 mL of the concentrated solution, add 100 μL of glacial acetic acid, that is, glacial acetic acid with a volume ratio of 20:1, and reflux at 100 °C for 20 hours. Adjust to neutral with sodium bicarbonate, recover the solvent under reduced pressure at 80°C to dryness...
Embodiment 2
[0064] Take the dried and mature fruit of Ligustrum lucidum, which is a plant of the genus Ligustrum in the family Oleaceae, crush it into a coarse powder, add 10 times the amount of water to reflux and extract 3 times, each time is 2 hours, combine the extracts, and recover the solvent under reduced pressure at 80 ° C to obtain Ligustrum Chaste seed concentrate.
[0065] Add glacial acetic acid with a volume ratio of 20:1 to the concentrate, and reflux at 100°C for 20 hours. Adjust to neutral with sodium bicarbonate, and recover the solvent to dryness under reduced pressure at 80°C to obtain salidroside hydrolyzate extract. Add a certain volume of distilled water to the hydrolyzate extract, so that the volume ratio of the amount of medicinal material to the dispersed solution is 1:2 (the amount of medicinal material refers to the weight of Ligustrum lucidum g: solution volume mL). Then centrifuge at a speed of 5000 rpm for 40 minutes, pour out the supernatant, which is ...
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