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Method for preparing neohesperidin in physiological fallen fruits of grapefruits by alcohol/salt double-water-phase system

A two-phase system, the technology of neohesperidin, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the difficulty and cost of improving the purification process, affect the purity of neohesperidin, and reduce drug residues. The problem of high alcohol content can ensure the purity and color, reduce the solvent content, and shorten the production cycle.

Active Publication Date: 2019-02-01
张家界普兰植物开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] (1) When extracting neohesperidin from Rutaceae plants, methanol or ethanol is often used for hot reflux extraction, the temperature is above 85°C, and there is The dissolution of a large amount of flavonoids such as naringin and hesperidin seriously affects the purity of neohesperidin and greatly increases the difficulty and cost of the subsequent purification process;
[0004](2) During the extraction process, a multifunctional extraction tank is used for reflux extraction, and percolation must be used during extraction. After the extraction, the alcohol content of the dregs is extremely high. Causes a huge waste of solvents, and alcohol-containing drug residues are also a major source of danger
[0005](3) During the extraction process, a large amount of steam is required for heating, which has a high risk factor, high energy consumption, and high production costs
The strong alkaline wastewater produced in the production process caused great environmental pollution, requiring a large amount of isovanillin as a reactant to ensure the conversion rate of naringin, thus increasing the production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] S1: Take 550 kg of dried pomelo physiological fruit drop, and transport it to the crushing machine room;

[0030] S2: The dried fruit in S1 is crushed and ground to 100 mesh to 300 mesh with a hammer mill and a wood flour machine successively, and 500 kg is taken for use;

[0031] S3: Add 2 cubic meters of deionized water to the liquid mixing tank, and weigh 400 kg of food-grade NaH 2 PO 4 Inorganic salt, fully stirred and dissolved, so that the mass fraction is 20% (w / w), after fully dissolved, measure 2 cubic meters of 70% isopropanol to form about 4 cubic meters of isopropanol / NaH 2 PO 4 Inorganic salt two-phase aqueous system, ph=5.1;

[0032] S4: Pump all the two-phase aqueous system in S3 into the extraction tank, add 500 kg of pomelo fruit dry powder in S2, turn on the mechanical stirring, control the rotation speed at 60 rpm, heat reflux extraction for 2.5 hours, and control the temperature at 55°C;

[0033] S5: The material after extraction is pumped into a l...

Embodiment 2

[0040] S1: Take 1080 kg of dried pomelo physiological fruit drop, and transport it to the crushing machine room;

[0041] S2: The dried fruit in S1 is crushed and ground to 100-300 mesh with a hammer mill and a wood flour machine successively, and 1000 kg is taken for use;

[0042] S3: Add 3 cubic meters of deionized water to the liquid mixing tank, and weigh 600 kg of food-grade NaH 2 PO 4 Inorganic salts, fully stirred and dissolved, so that the mass fraction is 20% (w / w), after fully dissolved, measure 3 cubic meters of 70% isopropanol to form about 10 cubic meters of isopropanol / NaH 2 PO 4 Inorganic salt two-phase aqueous system, ph=4.7;

[0043] S4: Pump all the two-phase aqueous system in S3 into the extraction tank, add 1000 kg of dried pomelo fruit powder in S2, turn on the mechanical stirring, control the rotation speed at 65 rpm, heat reflux extraction for 3 hours, and control the temperature at 57°C;

[0044] S5: The material after extraction is pumped into a li...

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Abstract

The invention belongs to the technical field of extraction of plant ingredients, and discloses a method for preparing neohesperidin in physiological fallen fruits of grapefruits by an alcohol / salt double-water-phase system. The method comprises the following steps: collecting dry grapefruit physiological fallen fruits; crushing the dry grapefruit physiological fallen fruits; pulverizing the dry grapefruit physiological fallen fruits; preparing and constructing a double-water-phase system; carrying out hot dip extraction; carrying out separation and phase splitting by a liquid-liquid-solid three-phase disc separating machine; concentrating; carrying out water sedimentation crystallization and filtering; carrying out ultra-filtration film assisted hot water recrystallization purification; carrying out cooling crystallization; and carrying out drying and packing. Advanced processes such as dip extraction through isopropanol / NaH2PO4 inorganic salt double-water-phase system, ultra-filtration film assisted hot water recrystallization purification and the like are adopted, and the whole process has the advantages of short production period, mild extracting conditions, simplicity and convenience in operation, high selectivity to target products, good product quality, small amount of waste water, easiness in treatment and the like, the yield of the prepared neohesperidin reaches 5.7%, and the HPLC content is greater than or equal to 95%.

Description

technical field [0001] The invention specifically relates to a method for preparing neohesperidin in grapefruit physiological drop by an alcohol / salt two-phase system, and belongs to the technical field of plant component extraction. Background technique [0002] Neohesperidin is a flavonoid extracted from natural citrus, grapefruit and other plants. Neohesperidin (Neohesperidin) is a kind of dihydroflavonoid compound, and its structural analysis shows that it is composed of 3,5,7-trihydroxyl-4'-methoxy flavone with a glycoside ligand and a rhamnosyl ligand. Glycosides composed of two units of glycosyl β-1,2-glucose. Because neohesperidin has activities such as scavenging free radicals, promoting gastric motility, lowering blood fat, anti-atherosclerosis, protecting the nervous system, anti-allergic, and anti-cancer, it has a wide range of uses in medicine; neohesperidin is also a An important intermediate that can be transformed into its derivative Neohesperidin Dihydroch...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/08
CPCC07H1/08C07H17/07
Inventor 李立刘磊磊齐克红
Owner 张家界普兰植物开发有限公司
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