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Method for rapidly extracting chalcone from fresh ashitaba

A chalcone and fresh technology, applied in the field of separation and purification of natural products, can solve the problems of eutrophication of phosphorus-containing wastewater, a large amount of organic solvents, and large safety hazards, so as to improve the extraction rate, avoid eutrophication pollution, The effect of increasing the extraction rate

Inactive Publication Date: 2014-03-26
QINGDAO UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example: patent CN201010299189.0 uses dry leaves as raw materials, and obtains chalcone through multiple extractions of ethanol, ethyl acetate, chloroform-methanol mixture and two column separations. This method not only has a large number of organic solvents and a large amount of use, but also The two column separations lead to low yield, long time consumption and low efficiency; patent CN201010127425.0 uses dry Ashitaba powder as raw material, extracts and recrystallizes with organic solvents such as isoamyl alcohol, acetone, chloroform, and isopropyl ether. In this production process, organic solvents such as flammable and explosive acetone, chloroform, and isopropyl ether are used, which not only cause great pollution, but also have great potential safety hazards; patent CN201110218657.1 uses petroleum ether, acetone, ethyl acetate and other The preparation of chalcones by extracting inorganic salts such as ammonium sulfate, dipotassium hydrogen phosphate, and potassium phosphate not only has a long process and many organic solvents, but also the discharge of a large amount of phosphorus-containing wastewater will cause eutrophication of the water body; the invention patent CN200910266615.8 directly adopts the bright day Leaves are used as raw materials, which simplifies the process steps, but the preparation process still uses organic solvents such as ethyl acetate, acetonitrile, and dimethyl sulfoxide, and the pollution problem has not been solved.

Method used

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  • Method for rapidly extracting chalcone from fresh ashitaba
  • Method for rapidly extracting chalcone from fresh ashitaba
  • Method for rapidly extracting chalcone from fresh ashitaba

Examples

Experimental program
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Effect test

Embodiment 1

[0042] The present invention, a kind of method for rapidly extracting chalcone from fresh and bright Japanese leaves, comprises the following steps:

[0043] Step 1: prepare compound enzyme, weigh and prepare according to the mass ratio of cellulase, dextranase and phytase as 8:2:1, and set aside;

[0044] Step 2: Weigh 1kg of fresh sun leaves, first cut and pulverize, then add 3 times the volume of water to homogenate; pour the homogenate into the extraction tank;

[0045] Step 3: Add 1 g of the compound enzyme prepared in Step 1 to the extraction tank, and stir evenly; adjust the pH to 5.0, and perform enzymatic hydrolysis at 35°C for 40 minutes; filter, and collect the filtrate as Filtrate 1;

[0046] Step 4: Add tetrachloroaluminate (1-ethyl-3-methyl) imidazole solution to filtrate one, the volume of tetrachloroaluminate (1-ethyl-3-methyl) imidazole solution and filtrate one The ratio is 2.5:1, extract at room temperature for 1 hour, filter and collect the filtrate to obt...

Embodiment 2

[0050] The present invention, a kind of method for rapidly extracting chalcone from fresh and bright Japanese leaves, comprises the following steps:

[0051] Step 1: prepare the compound enzyme, weigh and prepare according to the mass ratio of cellulase, dextranase and phytase of 7:3:2, and set aside;

[0052] Step 2: Weigh 1kg of fresh sun leaves, first cut and pulverize, then add 3 times the volume of water to homogenate; pour the homogenate into the extraction tank;

[0053] Step 3: Add 50 g of the compound enzyme prepared in Step 1 to the extraction tank, and stir evenly; adjust the pH to 6.0, and perform enzymatic hydrolysis at 40°C for 60 minutes; filter, and collect the filtrate as Filtrate 1;

[0054] Step 4: Add tetrachloroaluminate (1-ethyl-3-methyl) imidazole solution to filtrate one, the volume of tetrachloroaluminate (1-ethyl-3-methyl) imidazole solution and filtrate one The ratio is 3.5:1, extract at room temperature for 2 hours, filter and collect the filtrate ...

Embodiment 3

[0058] The present invention, a kind of method for rapidly extracting chalcone from fresh and bright Japanese leaves, comprises the following steps:

[0059] Step 1: prepare the compound enzyme, weigh and prepare according to the mass ratio of cellulase, glucanase and phytase of 5:5:1.5, and set aside;

[0060] Step 2: Weigh 1 kg of fresh sun leaves, first cut and pulverize, then add 5 times the volume of water to homogenate; pour the homogenate into the extraction tank;

[0061] Step 3: Add 20 g of the compound enzyme prepared in Step 1 to the extraction tank, and stir evenly; adjust the pH to 6.0, and perform enzymatic hydrolysis at 38°C for 50 minutes; filter, and collect the filtrate as Filtrate 1;

[0062] Step 4: Add tetrachloroaluminate (1-ethyl-3-methyl) imidazole solution to filtrate one, the volume of tetrachloroaluminate (1-ethyl-3-methyl) imidazole solution and filtrate one The ratio is 3:1, extract at room temperature for 1.5h, filter and collect the filtrate to ...

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PUM

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Abstract

The invention discloses a method for rapidly extracting chalcone from fresh ashitaba and belongs to the technical field of separation and purification of natural products. The method comprises the following steps: crushing a proper amount of fresh ashitaba, and homogenizing to obtain homogenate; adding composite enzyme into the homogenate, sufficiently stirring, filtering and collecting a filtrate 1; adding a tetrachloroaluminic acid (1-ethyl-3-methyl) imidazole solution into the filtrate 1, extracting for 1-2h at room temperature, filtering and collecting a filtrate 2; performing chromatographic separation on the filtrate 2 by using a polyamide chromatography column, eluting with ethanol, and drying at low pressure to obtain the chalcone. According to the invention, composite enzyme and the non-volatile tetrachloroaluminic acid (1-ethyl-3-methyl) imidazole solution are selected to replace the conventional volatile organic solvents, so that harms of the volatile organic solvents are eliminated to the maximum extent and safety risks are eliminated; the pure chalcone prepared by the method has the purity of more than 96% and the yield of more than 93%.

Description

technical field [0001] The invention belongs to the technical field of separation and purification of natural products, and in particular relates to a method for cleanly and rapidly extracting chalcones from fresh sun leaves. Background technique [0002] Chalcone (chalcone) refers to a class of natural compounds containing 1,3-diphenylpropenone structure in the molecule, which exists in large quantities in the roots, leaves and bark of various medicinal plants such as licorice and safflower, and its molecules The structure is flexible, and it can be combined with a variety of receptors, showing various biological activities. It has been reported that it has anti-tumor, anti-parasitic, anti-HIV, anti-bacterial, anti-inflammatory, anti-platelet aggregation and other effects. [0003] Angelica keiskei Koidzumi (Angelica keiskei Koidzumi), also known as Ashitaba, Mingyue grass, Hachijo grass, etc., is native to Japan’s Hachijo Island, Miura Peninsula and other coastal areas. ,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/796C07C45/78
CPCC07C45/78C07C49/796
Inventor 李子超钟进义
Owner QINGDAO UNIV
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