Method for extracting high-purity hesperetin from immature bitter orange
A high-purity hesperetin technology, which is applied in the field of extracting high-purity hesperetin from Citrus aurantium, can solve the problems of many intermediate links, high production cost, and long production cycle, and achieve short production cycle, low cost and low cost Effect
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Embodiment 1
[0021] Step 1, 1 kg of Citrus aurantium is pulverized and extracted three times with 85% ethanol with a mass concentration of reflux, the ethanol consumption of three times of reflux extraction is 20 times of the quality of Citrus aurantium, the reflux extraction time is 2 hours, and the filtrates are combined three times after filtration, The combined filtrate was concentrated under reduced pressure to a concentrated solution with a specific gravity of 1.02;
[0022] Step 2, adding sulfuric acid (or hydrochloric acid) to the concentrated solution described in step 1 to obtain a mixed solution, hydrolyzing the mixed solution for 5 hours at a temperature of 98° C., cooling to room temperature naturally, and filtering the obtained filter residue with The temperature is 80 ℃, and the soft water with hardness not more than 17.1 mg / L is washed and centrifuged to remove the supernatant, and the washing and centrifugation are repeated 3 times to obtain the crude product of hesperetin;...
Embodiment 2
[0026] Step 1, 1 kg of Citrus aurantium is pulverized and extracted three times with 95% ethanol with a mass concentration of reflux, the amount of ethanol used for three times of reflux extraction is 10 times that of Citrus aurantium quality, and the reflux extraction time is 1 hour, after filtering, the three filtrates are combined, Concentrating the combined filtrate under reduced pressure to a concentrated solution with a specific gravity of 1.0;
[0027] Step 2, add sulfuric acid (or hydrochloric acid) to the concentrated solution described in step 1 to obtain a mixed solution, hydrolyze the mixed solution for 3 hours at a temperature of 120° C., filter it after naturally cooling to room temperature, and use the filter residue obtained by filtering The temperature is 100 DEG C, and the hardness is not more than 17.1mg / L soft water washes and centrifuges to remove the supernatant to obtain the crude hesperetin; the mass concentration of sulfuric acid (or hydrochloric acid) ...
Embodiment 3
[0031] Step 1, after crushing 10kg Fructus Fructus Citrus Fructus Citrifolia, use mass concentration as 85% methanol reflux extraction three times, the amount of methanol used for the first refluxing extraction is 5 times of Fructus Fructus Aurantii quality, and the refluxing extraction time is 1.5 hours, the second refluxing extraction The methanol consumption is 8 times of the quality of Fructus Aurantii, and the reflux extraction time is 2 hours, and the methanol consumption of reflux extraction for the third time is 10 times of the quality of Fructus Aurantii, and the extraction time of reflux is 1 hour. Concentrate under reduced pressure to a concentrated solution with a specific gravity of 1.06;
[0032] Step 2, add hydrochloric acid (or sulfuric acid) to the concentrated solution described in step 1 to obtain a mixed solution, hydrolyze the mixed solution for 10 hours at a temperature of 90° C., filter it after naturally cooling to room temperature, and use the filter re...
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