Extraction and isolation experiments of rutinosides
This experimental method was obtained from the official website of the Fourth Military Medical University
Operation method
Extraction and isolation experiments of rutinosides
Principle
Rutin, also known as rutinoside, is widely found in the plant world, with the highest content in acacia rice (about 10%), which can be used as the raw material for extracting rutin. Rutin can increase the density and elasticity of capillaries, can be used for the treatment of capillary hemorrhage and arteriosclerotic hypertension, but also for the treatment of radiation-induced hemorrhagic syndrome. Rutin is a light yellow powder or very fine needle-like crystals, containing three molecules of water of crystallization, melting point 174 ° C ~ 178 ° C, anhydrous material melting point 188 ° C. The solubility in cold water is 1:10000, in hot water is 1:200, in cold ethanol is 1:650, in hot ethanol is 1:60, soluble in pyridine, glycerol, propylene glycol, glacial acetic acid or alkaline solution, insoluble in benzene, ether, chloroform. This experiment is the use of rutin molecular structure has more than one phenolic hydroxyl, weak acidity, soluble in alkaline solution, plus acid acidification can be precipitated rutin crystals, so that the extraction of alkali acid precipitation method.
Materials and Instruments
Sophora japonica Concentrated hydrochloric acid 1% sodium hydroxide solution Aluminum trichloride-ethanol solution Magnesium powder 70% ethanol Move 1. Rutin extraction Caveat 1. In this experiment, the rue glucoside was extracted directly from acacia rice with boiling water, the yield was stable and the operation was simple. 2. Before extraction, the acacia rice should be slightly crushed, so that the rue glucoside is easy to be put forward by hot water. 3. Use concentrated hydrochloric acid to adjust pH 4 ~ 5, do not over-acidification, such as pH value is too low, will reduce the yield of rue glucoside. For more product details, please visit Aladdin Scientific website.
Mastic bowl, funnel, filter paper, beaker, filter extraction device, tray balance, weighing paper, zeolite, skimmed cotton.
Weigh 20 grams of acacia rice, crushed, placed in 500 ml beaker, add 200 ml of boiling distilled water, heating and boiling for 30min, in time to replenish the loss of water. Pour out the supernatant while hot, filtered with cotton wool, dregs of the same operation with water and then extracted again, filtered while hot. Combine the two filtrates, adjust the pH 4-5 with hydrochloric acid, and leave overnight to precipitate crystals. Filtering, filter cake with a small amount of distilled water to wash 2 to 3 times, pumped dry, at room temperature and dry naturally, the crude rue glucoside.
2. Refinement
Take 2g of crude rue glucoside, placed in 500ml beaker, add distilled water 400ml, heating and boiling until all the rue glucoside dissolved, while hot filtration. The filtrate is placed overnight, can be precipitated crystals, filtration, natural drying in the air or 60 ℃ ~ 70 ℃ drying, to get the refined rue glucoside, weighing, calculating the yield.
3. Chemical identification
(1) salt reaction: take a little rue glucoside in a test tube, add 2ml of water and shake, observe any changes in the test tube. Add a few drops of 1% sodium hydroxide solution, shaking, it dissolves into a yellow clear solution. Then add a few drops of 1% hydrochloric acid solution, the yellow color becomes lighter, the solution from clear to turbid.
(2) Hydrochloric acid - magnesium powder test: take a little rue glucoside in a test tube, add 2 ml of ethanol, heat in a water bath to dissolve, add 2 to 3 drops of concentrated hydrochloric acid, and then add a little magnesium powder, that is, to produce a violent reaction, the solution gradually changed from yellow to red.
(3) Aluminum trichloride test: take a little rue glucoside, placed in a test tube, add ethanol 1 ~ 2ml, heated in a water bath to dissolve, add 1% aluminum trichloride - ethanol solution 2 ~ 3 drops, the solution is bright yellow.