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Method for separating high-purity hesperidin, neohesperidin, naringin and synephrine from fructus aurantii Immaturus

A new high-purity technology for neohesperidin, applied in chemical instruments and methods, preparation of organic compounds, preparation of sugar derivatives, etc., can solve the problem of low purity and yield of hesperidin, neohesperidin and synephrine , did not mention the separation method of naringin in Fructus Fructus Fructus Aurantium, the purity of the active ingredients in Fructus Fructus Fructus Fructus Fructus is not high, and achieved the effect of easy industrial production, simple operation and high purity

Inactive Publication Date: 2016-12-14
JIANGXI HAIFU BIOENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the purity of the active ingredients of Fructus Fructus Aurantium prepared is not high, it is a mixture of various substances, and thorough separation and purification have not been achieved.
[0005] Chinese patent CN105399787A discloses a method for extracting hesperidin, neohesperidin and synephrine from Fructus Aurantium, which extracts Fructus Fructus with ethanol, and repeatedly processes the extract by anion, macroporous resin and alkaline acid, but The purity and yield of hesperidin, neohesperidin and synephrine are low, and there is no mention of the separation method of naringin in Citrus aurantium

Method used

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Effect test

Embodiment 1

[0025] This embodiment includes the following steps:

[0026] (1) Enzymatic hydrolysis: 100 kg of Citrus aurantium (10.50% hesperidin content, 8.31% neohesperidin content, 6.23% naringin content, and 1.55% synephrine content) are crushed, infiltrated with 350kg water, and 0.35kg is added. Pectinase, enzymatic hydrolysis for 24 hours; (2) Extraction: add 2800kg of water to the enzymatically hydrolyzed raw materials, extract at 80°C for 2.5 hours, filter and cool to obtain a water extract, and water extract residue for use; (3) membrane separation : Filter the water extract with a nanofiltration membrane with a molecular weight cut-off of 800 to obtain the permeate and the retentate; (4) Separation of synephrine: absorb the permeate of the nanofiltration membrane with an anionic resin, and use a 2.5bv concentration as 1% ammonia is hydrolyzed and absorbed, concentrated, and recrystallized with dichloromethane to obtain synephrine 1.39kg, purity 98.77wt%, yield 89.68%; (5) Separatio...

Embodiment 2

[0028] This embodiment includes the following steps:

[0029] (1) Enzymatic hydrolysis: 100 kg of Citrus aurantium (10.50% hesperidin content, 8.31% neohesperidin content, 6.23% naringin content, and 1.55% synephrine content) are crushed, infiltrated with 400 kg of water, and 0.2 kg is added Pectinase, enzymatic hydrolysis for 20 hours; (2) Extraction: add 2500kg of water to the raw materials after enzymatic hydrolysis, extract for 2 hours at 70°C, filter and cool to obtain water extract, water extract residue for later use; (3) membrane separation : Filter the water extract with a nanofiltration membrane with a molecular weight cut-off of 600 to obtain a permeate and a retentate; (4) Separation of synephrine: absorb the permeate from the nanofiltration membrane with an anionic resin and use 2bv with a concentration of 1.5 % Ammonia is hydrolyzed and absorbed, concentrated, and refined by recrystallization of petroleum ether to obtain synephrine 1.3kg, purity 98.65wt%, yield 83.8...

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Abstract

The invention discloses a method for separating high-purity hesperidin, neohesperidin, naringin and synephrine from fructus aurantii Immaturus, and relates to a method for extraction of effective components of traditional Chinese medicines. The method includes the following steps: (1) enzymolysis, (2) extraction, (3) membrane separation, (4) synephrine separation, (5) naringin separation, (6) neohesperidin separation, and (7) hesperidin separation. The method has the advantages that the method overcomes the shortcomings in prior art, provides a new effective method which is easy to industrially produce, and is capable of combined extraction and separation various effective components in the fructus aurantii Immaturus, the method has the advantages of simple operation, high extraction rate, and high purity of the effective components, and the effective components all are separated, and easy to use.

Description

Technical field [0001] The present invention relates to a method for extracting effective ingredients of traditional Chinese medicine, in particular to a method capable of jointly extracting and separating multiple effective ingredients from Fructus Aurantii. Background technique [0002] Citrus aurantium is the dried young fruit of the Rutaceae plant Lime and its cultivars or sweet orange. Traditional Chinese medicine is used to treat stagnation and internal stagnation, fullness of swelling and pain, heavy diarrhea, obstruction of stool, phlegm stagnation and air blockage, chest pain, Chest, drooping organs. The effective ingredients of Fructus Aurantii include volatile oil, alkaloids and various glycosides. The main components of volatile oil are d-limonene and dextro-linalool; the main components of alkaloids are synephrine and N-methyltyramine; the glycosides are mainly hesperidin, neohesperidin, naringin, wild Anacardin, honeysuckle, etc. The various effective ingredients...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/08C07C213/10C07C215/60
CPCC07H17/07C07C213/10C07H1/08
Inventor 李伟龙伟岸黄华学
Owner JIANGXI HAIFU BIOENG
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