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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

Active Publication Date: 2012-05-02
XIAN XIAOCAO BOTANICAL DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, it mainly comes from the hydrolysis of hesperidin (Hesperidin), which mainly utilizes acid to hydrolyze hesperidin, and also uses enzyme method to hydrolyze it, but the production cost of hesperidin is relatively high with hesperidin as raw material, and the intermediate link Many, longer production cycle

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The invention discloses a method for extracting high-purity hesperetin from immature bitter orange, which comprises the following steps: 1. pulverizing immature bitter orange, extracting with alcohol solvent under reflux three times, filtering, merging the three filtrates, and concentrating; 2. adding inorganic acid into the concentrated solution for hydrolysis, naturally cooling to room temperature, filtering, washing the filter residues, and centrifugalizing to obtain a crude hesperetin product; and 3. dissolving the crude hesperetin product in ethanol, adding activated carbon to decolorize under reflux, filtering, concentrating, crystallizing, filtering, and drying the filtered solid matter to obtain the hesperetin crystals of which the mass purity is not lower than 95%.By using the immature bitter orange as the raw material for extraction, hydrolysis and refinement, compared with the traditional technique of extracting hesperetin from hesperidin, the invention reduces the intermediate links, lowers the production loss, enhances the production yield of hesperetin, lowers the production cost, and eliminates the hesperidin refinement, drying and other links in the original production process, thereby greatly shortening the production cycle.

Description

technical field [0001] The invention belongs to the technical field of extraction of plant effective components, and in particular relates to a method for extracting high-purity hesperetin from Citrus aurantium. Background technique [0002] Hesperetin (Hesperetin) is a class of natural flavonoids, widely found in fruits, flowers, food and other plant-derived substances. Hesperetin has a wide range of biological and pharmacological activities, and has been used in many fields such as organic chemistry, medicine, agronomy, and food. Modern medical research shows that hesperetin has a series of effects such as anti-oxidation, anti-inflammation, anti-virus, invigorating the stomach, antitussive, cardiovascular protection, nerve protection, and liver protection. Hesperetin has anti-inflammatory effects and can reduce sebum production. Effectively inhibit the growth of acne and be used to treat acne; as a biological antioxidant, hesperetin has the effect of protecting osteoblast...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/32C07D311/40
Inventor 陈冲
Owner XIAN XIAOCAO BOTANICAL DEV
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