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Method for extracting high-purity neohesperidin from immature bitter orange

A new hesperidin, high-purity technology, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve the problems of high production cost, large one-time investment, large amount of ethanol, etc., and achieve low cost , Reduce energy consumption, less impurity content effect

Active Publication Date: 2016-11-09
HUNAN HUACHENG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, under these extraction and purification conditions, the purity of neohesperidin is only 71.8226%, and the amount of ethanol used in this technology is large, resulting in large-scale production with large one-time investment and high production costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Enzyme soaking: Crush 500g of dried fruit of Citrus aurantium into 10-30 meshes, soak in 1250mL of water, then add 0.125g of compound plant hydrolytic enzyme preparation, and enzymatically hydrolyze for 120min at 40°C to obtain enzymatic hydrolysis of Citrus aurantium;

[0038] (2) Heat leaching: add 3kg of water to the enzymatic hydrolyzed Fructus Citrus Fructus obtained in step (1), conduct countercurrent leaching at 80°C for 60 minutes, cool to 45°C, and carry out three-legged sedimentation centrifugation at 1200r / min. Filter to obtain 3020mL citrus citrus enzyme extract;

[0039] (3) Flocculation and impurity removal: keep 3020mL of the citrus citrus citrus enzyme extract solution obtained in step (2) in a water bath, add 6.0g of ferric chloride, stir, and flocculate at 45°C for 60min, then add 6.0g of quicklime, Stir, and at 45°C, after flocculation treatment for 60 minutes, perform decanter centrifugation at 3000r / min, then disc centrifugation at 6000r / min, fi...

Embodiment 2

[0044] (1) Enzyme soaking: Crush 500g of dried fruit of Citrus aurantium into 10-30 meshes, soak in 1500mL of water, then add 0.30g of compound plant hydrolytic enzyme preparation, and enzymatically hydrolyze for 150min at 45°C to obtain enzymatic hydrolysis of Citrus aurantium;

[0045] (2) Heat leaching: Add 3.5kg of water to the enzymolyzed Citrus aurantium obtained in step (1), continuously countercurrent leaching at 90°C for 90 minutes, cool to 50°C, and carry out three-legged sedimentation centrifugation at a rate of 1200r / min. Filter to obtain 3480mL citrus citrus enzyme extract;

[0046] (3) Flocculation and impurity removal: Incubate 3480mL of the citrus citrus citrus enzyme extract solution obtained in step (2) in a water bath, add 8.0g of flocculated ferric chloride, stir, and flocculate at 50°C for 70min, then add 8.0g of quicklime , stirred, at 50°C, after flocculation treatment for 70 minutes, decanter centrifugation was carried out at a speed of 3000r / min, and d...

Embodiment 3

[0051] (1) Enzyme soaking: crush 500g of dried fruit of Citrus aurantium into 10-30 meshes, soak in 1700mL of water, then add 0.50g of compound plant hydrolytic enzyme preparation, and enzymatically hydrolyze for 180min at 50°C to obtain enzymatic hydrolysis of Citrus aurantium;

[0052] (2) Heat leaching: Add 4.0kg of water to the enzymatically hydrolyzed Citrus aurantium obtained in step (1), continuously countercurrent leaching at 95°C for 120min, cool to 55°C, and carry out three-legged sedimentation centrifugation at a rate of 1200r / min. Filter to obtain 4180mL citrus citrus enzyme extract;

[0053] (3) Flocculation and impurity removal: keep 4180mL of the citrus citrus citrifolia and enzyme extract solution obtained in step (2) in a water bath, add 12.0g of ferric chloride, stir, and flocculate at 55°C for 80min, then add 8.0g of quicklime, Stir, and at 55°C, after flocculation treatment for 80 minutes, perform decanter centrifugation at a rate of 3000r / min, then disc ce...

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Abstract

The invention discloses a method for extracting high-purity neohesperidin from an immature bitter orange. The method comprises the following steps: (1) crushing and impregnating an immature bitter orange raw material in water, adding a compound plant-hydrolase preparation, and performing enzymatic decomposition to obtain an enzymatically decomposed immature bitter orange; (2) performing heating extraction, cooling, centrifugation and filtration on the enzymatically decomposed immature bitter orange to obtain enzymatic immature bitter orange extract; (3) performing water bath heat preservation on the enzymatic immature bitter orange extract, adding a flocculating agent for flocculation treatment, and performing centrifugation and filtration to obtain immature bitter orange flocculation liquid; (4) performing nanofiltration, concentration and vacuum drying on the immature bitter orange flocculation liquid to obtain a neohesperidin crude product; (5) completely dissolving the neohesperidin crude product in an ethanol solution, performing strict filtration, and repeatedly performing cooling crystallization, washing and vacuum drying to obtain a high-purity neohesperidin product. The purity of the product obtained by the method can reach 98.6 percent, and the final yield is more than 90 percent; the method is simple in process, high in operability, low in energy consumption and cost, suitable for industrial production, small in ethanol residue amount, environment-friendly and safe.

Description

technical field [0001] The invention relates to a method for extracting high-purity neohesperidin, in particular to a method for extracting high-purity neohesperidin from Citrus aurantium which is suitable for industrial production. Background technique [0002] Citrus aurantium, belonging to the Rutaceae plant, is widely distributed in China. It is the traditional name for lime in China. In traditional Chinese medicine, as a traditional folk herbal medicine, Citrus aurantium is mainly used to enhance appetite and regulate qi (energy). In Italy, aurantium is also one of the traditional folk medicines since the 16th century, used to treat fevers such as malaria and as an antibacterial agent. Recent studies have confirmed that Citrus aurantium can replace ephedra in the treatment of obesity without adverse cardiovascular side effects. [0003] Modern studies have found that mature citrus aurantium contains hesperidin, naringin, synephrine, and N-methyltyramine. When the frui...

Claims

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Application Information

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IPC IPC(8): C07H1/08C07H17/07
CPCC07H1/08C07H17/07
Inventor 龙伟岸黄华学
Owner HUNAN HUACHENG BIOTECH
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