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Method for separating hesperetin from immature bitter oranges

A technology of hesperetin and citrus aurantium, which is applied in the direction of organic chemistry, can solve the problem of low utilization rate of hesperidin, and achieve the effects of full utilization, low production cost and high yield

Active Publication Date: 2021-11-16
HUNAN HUACHENG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method does not need to obtain high-content hesperidin products, and also omits the steps of hesperidin separation and purification, refining and drying, hesperidin extraction and concentration steps are still required. If the hesperidin extraction is not thorough, the hesperidin still underutilized

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039](1) Enzymolysis: Take 50kg of Fructus Citrifolia raw material, crush it until the particle size is 1-2mm, and set aside; dissolve 0.5kg of ligninase in 50 L of pure water, adjust the pH value to 4.5, and then add it to the crushed Fructus Citrus aurantium In the real raw material, stir and mix evenly, and enzymolyze at room temperature for 24 hours to obtain the enzymatic hydrolyzate of Citrus citrus;

[0040] (2) Pressurized hydrolysis: put the citrus citrus enzymolyzate obtained in step (1) into a high-pressure reactor, add 1000 L of acid water (dilute hydrochloric acid with a mass percentage concentration of 2.0%), and heat it at a temperature of 110°C and a pressure of Pressurized hydrolysis under the condition of 0.15Mpa for 3 hours, after the hydrolysis was completed, the reaction solution was cooled to room temperature, centrifuged and filtered, the filter cake was collected, washed with water until neutral, and the filter cake was dried to obtain Citrus aurantium ...

Embodiment 2

[0046] (1) Enzymolysis: take 50kg of Fructus Citrifolia raw material, crush it until the particle size is 1-2mm, and set aside; dissolve 1.2kg of ligninase in 100 L of pure water, adjust the pH value to 5.0, and then add it to the crushed Fructus Citrifolia In the real raw material, stir and mix evenly, and enzymolyze at room temperature for 20 hours to obtain the enzymatic hydrolyzate of Fructus Citrus Fructus;

[0047] (2) Pressurized hydrolysis: put the citrus citrus enzymolyzate obtained in step (1) into a high-pressure reactor, add 800 L of acid water (dilute hydrochloric acid with a mass percentage concentration of 1.6%), and heat it at a temperature of 120 °C and a pressure of Under the condition of 0.26Mpa, pressurize and hydrolyze for 2.5 hours. After the hydrolysis is completed, the reaction solution is cooled to room temperature, centrifuged and filtered, and the filter cake is collected. The filter cake is washed with water until neutral, and the filter cake is drie...

Embodiment 3

[0053] (1) Enzymolysis: Take 50kg of Fructus Aurantium raw material, crush it to a particle size of 1-2mm, and set aside; dissolve 0.9kg of ligninase in 70 L of pure water, adjust the pH value to 4.7, and then add the crushed Fructus Fructus Aurantium Stir and mix the raw materials evenly, enzymatically hydrolyze at room temperature for 18 hours, and obtain the enzymatic hydrolyzate of Citrus aurantium;

[0054] (2) Pressurized hydrolysis: put the citrus aurantium enzymolyzate obtained in step (1) in a high-pressure reactor, add 900 L of acid water (dilute sulfuric acid with a mass percentage concentration of 0.8%), and heat it at a temperature of 107 °C and a pressure of Pressurized hydrolysis under the condition of 0.12Mpa for 2 hours, the hydrolysis was completed, the reaction solution was cooled to room temperature, centrifugally filtered, the filter cake was collected, the filter cake was washed with water until neutral, and the filter cake was dried to obtain Citrus auran...

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PUM

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Abstract

The invention discloses a method for separating hesperetin from immature bitter oranges. The method comprises the following steps: (1) enzymolysis: dissolving ligninase in water, adding into a crushed immature bitter orange raw material, uniformly mixing, and carrying out enzymolysis at room temperature to obtain an immature bitter orange zymolyte; (2) pressurized hydrolysis: putting the immature bitter orange zymolyte into a high-pressure reaction kettle, adding acid water, heating, and carrying out pressurized hydrolysis to obtain a reaction solution; cooling the reaction solution to room temperature, centrifugally filtering, collecting a filter cake, washing the filter cake to be neutral with water, and drying the filter cake to obtain immature bitter orange hydrolysate; (3) reflux extraction: performing reflux extraction on the immature bitter orange hydrolysate by using an organic solvent to obtain an organic solvent extracting solution; (4) decoloring; and (5) concentrating and crystallizing to obtain a hesperetin product. The method is simple and convenient to operate, low in equipment requirement and low in production cost, and the hesperetin product is high in hesperetin content and high in yield.

Description

technical field [0001] The invention relates to a method for isolating hesperetin, in particular to a method for isolating hesperetin from Citrus aurantium. Background technique [0002] Hesperetin (hesperetin) belongs to dihydroflavonoids and is the main active ingredient in the fruit of Citrus L. in the Rutaceae family. Hesperetin does not exist in the form of hesperetin in nature, but mainly exists in the form of hesperidin (hesperidin). Hesperetin is the glycosyl ligand of hesperidin. Its structure contains ketone carbonyl, ether, methoxy and multiple phenolic hydroxyl groups. It is widely used in many fields such as organic chemistry, medicine, agronomy, and food. [0003] Hesperetin will not accumulate in any organs, and it is safe to use without obvious side effects. Early studies on the pharmacological effects of hesperetin mainly focused on antibacterial, anti-inflammatory, anti-oxidant, anti-viral, anti-allergic, regulating blood lipids, enhancing immunity and an...

Claims

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Application Information

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IPC IPC(8): C07D311/32C07D311/40
CPCC07D311/32C07D311/40
Inventor 李伟黄华学贺进军黄俊宋谷良江小龙吴国亮
Owner HUNAN HUACHENG BIOTECH