A method for synergistically extracting active components in mulberry branches (leaves) by strengthening hydrothermal reaction with solid acid
A hydrothermal reaction and active ingredient technology, applied in separation methods, chemical instruments and methods, medical preparations containing active ingredients, etc., can solve the problems of long time consumption, large amount of petroleum ether and ethanol, and damage to plant cell walls
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Embodiment 1
[0022] (1) Raw material pretreatment
[0023] The picked fresh mulberry leaves were dried in an oven at 60°C for 5 hours, and the dried mulberry leaves were pulverized into powder by a pulverizer, sieved with 80 mesh, put into sealed bags, and set aside.
[0024] (2) Solid acid enhanced hydrothermal reaction treatment of raw materials
[0025] After step (1) is completed, first weigh 2g of pretreated mulberry leaf powder into the hydrothermal reaction kettle, then add 5‰ of the mass of mulberry leaves (g), that is, 0.01g of phosphotungstic heteropolyacid, and finally The ratio of water ethanol volume (ml) to mulberry leaf powder mass (g) is 9:1, measure 18ml of absolute ethanol and pour it into the hydrothermal reaction kettle. Then, the reaction kettle was put into an oven at 180° C. to react for 110 minutes.
[0026] (3) Analysis and detection of active ingredients
[0027] After step (2) is completed, take out the reaction kettle and cool it to room temperature, pour it ...
Embodiment 2
[0031] A method for synergistically extracting active ingredients in mulberry branches (leaves) by solid acid-enhanced hydrothermal reaction, the same as in Example 1, wherein:
[0032] In step (1), the oven temperature is 50°C, the drying time is 6 hours, and the sieve is 60 mesh.
[0033]In step (2), the mass (g) of phosphotungstic heteropolyacid is 4‰ of the mass (g) of mulberry leaf, the ratio of absolute ethanol (ml) to the mass (g) of mulberry leaf powder is 7:1, and the reaction The temperature is 170° C., and the reaction time is 130 minutes.
[0034] In step (3), the rotation speed is 2000r / min, and the centrifugation time is 20min. The ratio of acetonitrile (ml) to water (ml) was 35:65, the temperature was 30°C, the injection volume was 5 μL, the flow rate was 0.8ml / min, and the peak area (mAu*s) was 19738.334.
[0035] In step (4), when the vacuum pressure is 0.4Mpa and the temperature is 80°C, the ratio of the mass (g) of the mulberry leaf extract product to the ...
Embodiment 3
[0037] A method for synergistically extracting active ingredients in mulberry branches (leaves) by solid acid-enhanced hydrothermal reaction, the same as in Example 1, wherein:
[0038] In step (1), the oven temperature is 70°C, the drying time is 4 hours, and the sieve is 100 mesh.
[0039] In step (2), the mass (g) of phosphotungstic heteropolyacid is 6‰ of the mass (g) of mulberry leaf, the ratio of absolute ethanol (ml) to the mass (g) of mulberry leaf powder is 11:1, and the reaction The temperature is 190° C., and the reaction time is 90 minutes.
[0040] In step (3), the rotational speed is 3000r / min, the centrifugation time is 15min; the ratio of acetonitrile (ml) to water (ml) is 50:50, the temperature is 40°C, the injection volume is 20μL, the flow rate is 1ml / min, the peak The area (mAu*s) is 18549.287.
[0041] In step (4), when the vacuum pressure is 0.6Mpa and the temperature is 100°C, the mass (g) of the mulberry leaf extract product: the volume (ml) ratio of ...
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