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Method for purifying neohesperidin

A new hesperidin and purification method technology, applied in the field of natural product separation, can solve the problems of difficult operation and difficult to obtain high-purity products, and achieve the effects of low pollution, high purity and low energy consumption

Inactive Publication Date: 2012-05-30
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing process is difficult to operate when the actual process is scaled up, and it is also difficult to obtain high-purity products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Crush the dried Fructus Aurantii raw material, take 50kg into the extraction tank, add 750kg water for reflux extraction for 2 hours, suction filter to obtain the extract, then add 500kg water for reflux extraction for 1 hour, combine the two extracts and add 80L ADS-17 macroporous resin column for adsorption , The flow rate is 100L / h, the adsorption is complete, wash the resin column with water to sugar-free color, then take 480L of 50% ethanol solution to elute the active ingredients, collect the eluate, add hollow fiber membrane ultrafiltration with a molecular weight cutoff of 3000, and control the inlet pressure of the ultrafiltration at 0.5-0.8Mpa, add a small amount of 50% ethanol solution for dialysis, collect the permeate and pressurize to recover the ethanol, the concentrated solution is left to crystallize for 12 hours, centrifuged to obtain 7.4kg of crude crystals, add 25L of 50% acetone to reflux to dissolve, filter by frame filter, filter The product was the...

Embodiment 2

[0020] Crush the dried Fructus Aurantii raw material, take 50kg into the extraction tank, add 500kg water for reflux extraction for 2 hours, suction and filter the extract, then add 500kg water for reflux extraction for 1 hour, combine the two extracts and add 90L LSA-20 macroporous resin column for adsorption , The flow rate is 120L / h, the adsorption is complete, wash the resin column with water to sugar-free color, then take 360L of 70% ethanol solution to elute the active ingredients, collect the eluent, add a hollow fiber membrane ultrafiltration with a molecular weight cutoff of 6000, and control the ultrafiltration inlet pressure at 0.5-0.6Mpa, add a small amount of 70% ethanol solution for dialysis, collect the permeate and pressurize to recover the ethanol. The concentrated solution is left to crystallize for 20 hours, centrifuged to obtain crude crystals of 8.6kg, add 35L 70% acetone to reflux to dissolve, filter by plate and frame filter, filter The product was refluxe...

Embodiment 3

[0022] Crush the dried Fructus Aurantii raw material, take 50kg into the extraction tank, add 600kg of water for reflux extraction for 2 hours, suction and filter to obtain the extract, then add 600kg of water for reflux extraction for 1 hour, combine the two extracts and add 90LAB-8 macroporous resin column for adsorption, Flow rate 110L / h, adsorption is complete, wash the resin column with water to sugar-free color, then take 450L of 60% ethanol solution to elute the active ingredients, collect the eluate, add a hollow fiber membrane ultrafiltration with a molecular weight cutoff of 10,000, and control the ultrafiltration inlet pressure at 0.5 -0.6Mpa, add a small amount of 60% ethanol solution for dialysis, collect the permeate and pressurize to recover ethanol, leave the concentrated solution to crystallize for 14 hours, centrifuge to obtain 9.2kg of crude crystals, add 39L 60% acetone to reflux to dissolve, filter by frame filter, filter out The product was then refluxed wi...

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PUM

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Abstract

The present invention relates to a method for purifying neohesperidin. The method comprises pulverizing dried Fructus Aurantii Immaturus, performing reflux extraction with 10-15 times amount of water for 2-3 times, filtering the obtained extractive solution, adsorbing via a macroporous resin column, eluting with water until the eluate has no sugar color, eluting with 4-6 times amount of 50-70% ethanol solution, collecting the eluate, ultrafiltering with an ultrafiltration membrane system, collecting the obtained filtrate, recovering ethanol under a reduced pressure, standing the obtained concentrated solution for crystallization, filtering out crystal, refluxing and dissolving with 3-6 times amount of 50-70% acetone, filtering, performing reflux dissolution and crystallization on filter residue with deionized water for 2-3 times, and drying crystal. The invention has low production cost and simple operation, and facilitates industrial production. The prepared neohesperidin has high purity.

Description

Technical field: [0001] The invention belongs to the field of natural product separation, and particularly relates to a method for purifying new hesperidin. Background technique: [0002] Neohesperidin is a flavonoid substance widely found in citrus fruits. Its chemical structure is a dihydroflavonoid glycoside structure, with a melting point of 240-243°C and a molecular weight of 610.6. It is almost insoluble in acetone, benzene, and chloroform. Slightly soluble in methanol, ethanol, hot glacial acetic acid, and easily soluble in dilute alkali solution and hot water. [0003] Neohesperidin has anti-inflammatory and antiviral effects, and is also a synthetic raw material for the sweetener Neohesperidin dihydrochalcone. [0004] Citrus aurantium is the dried young fruit of the rutaceae plant Lime and its cultivated varieties or sweet orange. It contains a lot of flavonoids, among which the content of neohesperidin is about 10%. [0005] Neohesperidin is mostly extracted from orange pe...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/08
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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