Method for simultaneously isolating and purifying chrysin-5-glucoside and chrysin from malus pumila

A technology for simultaneous separation of glucosides, applied in chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve the problems of single separation to obtain chrysin glycosides, the difficulty of separation of chrysin is increased, and the recovery rate of target products is low. Achieve the effect of easy industrial production, simple and easy operation, and short process cycle

Active Publication Date: 2020-04-28
GUANGXI INST OF BOTANY THE CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among these methods, there are mainly alcohol extraction polyamide column purification method, alcohol extraction macroporous adsorption resin enrichment solvent extraction method, water extraction macroporous adsorption resin purification method, water extraction alcohol precipitation method, etc., but the prior art either only focuses on Chrysin or chrysin glycosides are directly extracted from a raw material. When chrysin or chrysin glycosides exist in the raw material at the same time, the other one of chrysin or chrysin glycosides in the extract cannot be fully obtained; or directly The chrysin glucoside in the raw material is hydrolyzed into chrysin by acid and enzyme and then extracted and separated. Although the chrysin aglycone in the raw material can be fully obtained in this way, the acid and enzymatic hydrolysis process before extraction will also lead to other components in the raw material. A large number of by-products are produced due to the decomposition of chrysin, the difficulty of subsequent separation of chrysin in the extract is increased, the final recovery rate of the target product is low or the cost of separation and purification increases
In summary, the existing methods can only separate and obtain chrysin glycoside or chrysin from plants through simple macroporous adsorption resin column purification, and there is no simultaneous separation and purification of chrysin and poplar from one raw material. Related reports about glucoside

Method used

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  • Method for simultaneously isolating and purifying chrysin-5-glucoside and chrysin from malus pumila
  • Method for simultaneously isolating and purifying chrysin-5-glucoside and chrysin from malus pumila
  • Method for simultaneously isolating and purifying chrysin-5-glucoside and chrysin from malus pumila

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Take the branches of Malus doumeri (Bois) Chevalier), dry in the sun, pulverize, pass through a 20-mesh sieve, and collect the under-sieve as the extraction raw material; the content of chrysin-5-glucoside and chrysin in the extraction raw material Detected (HLPC method, the same below), they were 3.87% and 1.05% respectively;

[0029] 2) Put 5Kg of extraction raw materials in an extraction container, add 60v / v% ethanol equivalent to 8 times the weight of the raw materials, heat up to 70°C for ultrasonic extraction (ultrasonic power is 200W) for 1.0h, filter, and repeat the above conditions for the filter residue to extract 2 times, the filtrates were combined to obtain the extract;

[0030] 3) The obtained extract is concentrated in vacuum to an extract, and the obtained extract is dissolved with 15v / v% ethanol to a saturated solution, left to stand overnight, and the supernatant is taken for later use;

[0031] 4) Equilibrate the macroporous adsorption resin colum...

Embodiment 2

[0053] 1) Get the leaves of Malus doumeri (Bois) Chevalier), dry in the sun, pulverize, pass through a 20-mesh sieve, and collect the under-sieve as the extraction raw material; the content of chrysin-5-glucoside and chrysin in the extraction raw material is analyzed. Detection (HLPC method, the same below), respectively 4.43% and 1.07%;

[0054] 2) Put 5Kg of extraction raw materials in an extraction container, add 80v / v% methanol equivalent to 6 times the weight of the raw materials, heat up to 60°C for reflux extraction for 2.0h, filter, and repeat the extraction of the filter residue twice under the above conditions, and combine the filtrates to obtain Extraction solution;

[0055] 3) The obtained extract is concentrated in vacuum to an extract, and the obtained extract is dissolved with 10v / v% methanol to a saturated solution, left to stand overnight, and the supernatant is taken for later use;

[0056] 4) First equilibrate the macroporous adsorption resin column (resin ...

Embodiment 3

[0060] 1) Take the branches of Malus melliana (Hand.-Mazz.) Rehder), dry in the sun, pulverize, pass through a 40-mesh sieve, and collect the under-sieve as the extraction raw material; Chrysin-5-glucoside in the extraction raw material and chrysin content were detected, which were 3.34% and 1.21% respectively;

[0061] 2) Put 5Kg of extraction raw materials in an extraction container, add 80v / v% ethanol equivalent to 5 times the weight of the raw materials, reflux extraction for 2.0h, filter, repeat the extraction of the filter residue under the above conditions once, and combine the filtrates to obtain the extract;

[0062] 3) The obtained extract is concentrated in vacuum to an extract, and the obtained extract is dissolved with 25v / v% ethanol to a saturated solution, left to stand overnight, and the supernatant is taken for later use;

[0063] 4) Equilibrate the macroporous adsorption resin column (resin model is AB-8) with 3 times the column volume and 25v / v% ethanol firs...

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Abstract

The invention discloses a method for simultaneously isolating and purifying chrysin-5-glucoside and chrysin from malus pumila. The method comprises steps of taking branches and/or leaves of malus pumila as raw materials to obtain extracting solution; concentrating the extracting solution to obtain an extractum, dissolving the extractum with 5-30 v/v% of low-carbon alcohol or alkaline solution withpH>=8, taking supernatant, isolating and purifying the supernatant with a macroporous adsorption resin column, conducting gradient elution with low-carbon alcohol-water system, sectionally collectingfractions, and merging fractions rich in chrysin-5-glucoside and chrysin respectively and recycling a solvent to obtain the chrysin-5-glucoside and chrysin respectively. According to the method of the present invention, the chrysin-5-glucoside and chrysin are simultaneously isolated and purified with the simple macroporous adsorption resin column by using branches and/or leaves of malus pumila asraw materials for the first time, and the obtained chrysin-5-glucoside and chrysin have higher purity. The method of the present invention is simple and easy to operate, large in processing capacity,high in recovery rate, short in process cycle, low in production cost, and easy to industrialization.

Description

technical field [0001] The invention relates to a method for extracting and isolating active ingredients from plants, in particular to a method for simultaneously separating and purifying chrysin-5-glucoside and chrysin from ringworm. Background technique [0002] Ringo, which belongs to the Rosaceae Malus plant, has Taiwan Ringo (Malus doumeri (Bois) Chevalier), pointed mouth Ringo (Malus melliana (Hand.-Mazz.) Rehder) and light calyx Ringo (Malus leioc alycaS.Z.Huang) three. A closely related species, mainly distributed in my country's Jiangxi, Hunan, Fujian, Guangxi, Yunnan, Guizhou and Taiwan. The "Big Fruit Hawthorn" and "Guanghawthorn" commonly known in Guangxi, and the "Winter Pear" and "Huahong" commonly known in Hunan belong to Taiwan Ringo. [0003] Ringo is rich in bioactive ingredients such as polyphenols, flavonoids, and triterpenes. It has a wide range of pharmacological activities such as anti-cancer, lowering blood pressure, lowering lipids, anti-oxidation, p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08C07D311/30C07D311/40
CPCC07D311/30C07D311/40C07H1/08C07H17/07
Inventor 蔡爱华霍华珍谢运昌孙博李典鹏
Owner GUANGXI INST OF BOTANY THE CHINESE ACAD OF SCI
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