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Method for simultaneously extracting high-purity naringin and neohesperidin from fructus aurantii

A new hesperidin and naringin technology, applied in chemical instruments and methods, preparation of sugar derivatives, bulk chemical production, etc., can solve problems such as unfavorable small batch production, unexpected extraction rate, and lower extraction temperature. Achieve the effect of reducing the formation of impurities, low cost and high extraction rate

Active Publication Date: 2019-06-21
重庆市铜梁区子奇药材有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since naringin and neohesperidin are flavonoids containing phenolic hydroxyl groups and are sensitive to heat, the microwave-assisted extraction technology of naringin and neohesperidin in Fructus Fructus was studied, along with Soxhlet extraction and ultrasonic-assisted extraction. Compared with other methods, the extraction temperature is lowered, the thermal stability of flavonoids is ensured, and the extraction rate is improved, but the extraction rate is not expected, and the extraction process does not introduce too much about the purity of the extract, so it cannot be regarded as sweetness. Synthesis of Naringin Dihydrochalcone and Neohesperidin Dihydrochalcone Provides High Purity Raw Materials
[0012] In order to solve the problem of low purity of the above-mentioned extracts, Hu Changsheng et al. (Clinical Rational Drug Use, 2013, 6(11C), 58-60) used high-speed countercurrent chromatography to rapidly prepare high-purity naringin and neohesperidin from Fructus Aurantii , purity>99%,
Although high-purity naringin and neohesperidin can be obtained by this method, the current high-speed countercurrent chromatography can only achieve the preparation and separation of hundreds of milligrams or even tens of grams, and the amount of separation at one time is small, which is not conducive to the production of small batches.

Method used

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  • Method for simultaneously extracting high-purity naringin and neohesperidin from fructus aurantii

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1) Select Fructus Fructus Fructus Fructus Aurantii to dry, pulverize, and pass through a 60-mesh sieve; HPLC method determines that the contents of naringin and neohesperidin are 7.3% and 7.1% respectively; take 500g of the sieved material and put it into supercritical CO2 extraction In the extraction kettle of the instrument.

[0031] 2) Set the parameters of the extraction kettle in step 1), select the extraction temperature as 20°C, the extraction pressure as 20MPa, the extraction time as 1h, and the CO2 flow rate as 50kg / h, statically extract the volatile oil, and after solid-liquid separation, depressurize to obtain 7.0ml primary extract.

[0032] 3) Keep the citrus aurantium residue after extracting the volatile oil in step 2) in the extraction kettle, add 2.5L 80% ethanol as entrainer at a liquid-solid ratio of 5:1 (ml:g), select the extraction temperature at 40°C, and extract Pressure 40MPa, extraction time 1h and CO2 flow rate 20kg / h, statically extract naring...

Embodiment 2

[0037] 1) Select Fructus aurantii to dry, pulverize, pass through a 60-mesh sieve, and get 500g of the sieved material into the extraction kettle of the supercritical CO2 extractor;

[0038] 2) Set the parameters of the extraction kettle in step 1), select the extraction temperature to be 30°C, the extraction pressure to be 35MPa, the extraction time to be 2h, and the CO2 flow rate to be 60kg / h, to statically extract the volatile oil, and after solid-liquid separation, reduce pressure to obtain 8.0ml primary extract;

[0039] 3) Keep the citrus aurantium residue after extracting the volatile oil in step 2) in the extraction kettle, add 2.5L of 80% ethanol as an entrainer at a liquid-solid ratio of 5:1 (ml:g), select an extraction temperature of 50°C, and extract Pressure 50MPa, extraction time 2h and CO2 flow rate 30kg / h, statically extract naringin and neohesperidin, and collect the secondary extract after solid-liquid separation;

[0040] 4) concentrating the secondary extr...

Embodiment 3

[0044] 1) Select Fructus aurantii to dry, pulverize, pass through a 60-mesh sieve, and get 500g of the sieved material into the extraction kettle of the supercritical CO2 extractor;

[0045] 2) Set the parameters of the extraction kettle in step 1), select the extraction temperature as 40°C, the extraction pressure as 40MPa, the extraction time as 3h, and the CO2 flow rate as 80kg / h, statically extract the volatile oil, and after solid-liquid separation, depressurize to obtain 8.0ml primary extract;

[0046] 3) Keep the citrus aurantium residue after extracting the volatile oil in step 2) in the extraction kettle, add 2.5L of 80% ethanol as entrainer at a liquid-solid ratio of 5:1 (ml:g), select the extraction temperature at 60°C, and extract Pressure 60MPa, extraction time 3h and CO2 flow rate 40kg / h, statically extract naringin and neohesperidin, and collect the secondary extract after solid-liquid separation;

[0047] 4) concentrating the secondary extract in step 3) to dr...

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Abstract

The invention provides a method for simultaneously preparing high-purity naringin and neohesperidin from fructus aurantii. Essential oil in the fructus aurantii is extracted by a supercritical CO2 extraction technology at first, and then a naringin and neohesperidin crude extract mixture is extracted by the supercritical CO2 extraction technology. The crude extract mixture is separated and purified by macroporous adsorption resin to obtain the naringin and the neohesperidin. The method provided by the invention has the advantages of high extraction rate, high product purity, environmental friendliness and low cost, and is suitable for industrial production of high-purity naringin and neohesperidin.

Description

technical field [0001] The invention belongs to the technical field of extracting effective components from Fructus aurantii, and specifically relates to a method for simultaneously extracting high-purity naringin and neohesperidin from Fructus aurantii. Background technique [0002] The structural formula of naringin is as follows figure 1 As shown (wherein R: rhamnosyl), the naringin has anti-inflammatory, anti-virus, anti-cancer, anti-mutation, anti-allergic, anti-ulcer, analgesic, hypotensive activities, can lower cholesterol, reduce the risk of thrombus Formation can improve local microcirculation and nutrient supply, and can be used to produce drugs for preventing and treating cardiovascular and cerebrovascular diseases. Naringin is also a raw material for the synthesis of neohesperidin and naringin dihydrochalcone. [0003] The structural formula of neohesperidin is as follows figure 1 As shown (where R: rhamnosyl), the neohesperidin has activities such as scavengi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H1/08C07H17/07
CPCY02P20/54
Inventor 夏仕文谢光伟何从林徐红梅杨晓霞谢显奇林子力
Owner 重庆市铜梁区子奇药材有限公司
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