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Method for extracting isobavachalcone from fresh angelica keiskei

A new and fresh technology of isopsoralenchalcone, which is applied in the field of preparation of isopsoralenchalcone, can solve the problems that the preparation method has not been reported, and achieve the goal of reducing the difficulty of process control, saving energy, and having a single component Effect

Active Publication Date: 2015-09-23
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In the existing technology, the obtained chalcone product is the whole ketone product of Ashitaba, but there are 8 kinds of chalcone derivatives known in Ashitaba, a single chalcone, especially isopsoralen The preparation method of chalcone has no report at present

Method used

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  • Method for extracting isobavachalcone from fresh angelica keiskei
  • Method for extracting isobavachalcone from fresh angelica keiskei
  • Method for extracting isobavachalcone from fresh angelica keiskei

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] (1) Beat 1Kg fresh sun leaves, mix according to the ratio of the volume ratio of the slurry to the alcohol-water solution of 1:7, wherein the volume ratio of ethanol to water is 19:2, heat up to 72°C, stir and leaching for 3 hours, then filter , Obtain 7.5L filtrate A.

[0049] (2) Mix A and n-hexane at a ratio of 1:1 by volume, stir for 3 hours, remove chlorophyll impurities, let stand to separate, and take 7L of hydroalcoholic phase B.

[0050] (3) Mix B and saturated lime water at a volume ratio of 1:0.3 for 2 hours to remove tannin and other alkali-soluble impurities, and filter to obtain 8.5L of filtrate C.

[0051] (4) Mix C and ethyl acetate at a volume ratio of 1:0.5, then add 1.5 L of 10% sodium bicarbonate and shake for 4 hours to remove fat-soluble impurities to obtain 9.6 L of aqueous phase D.

[0052] (5) Replace the macroporous resin AB8 separation column on D for 1.5 hours, wash with water to remove small water-soluble molecules such as sugars, and final...

Embodiment 2

[0055] (1) Beat 1Kg fresh sun leaves, mix according to the volume ratio of slurry and alcohol-water solution is 1:7, wherein, the volume ratio of methanol to water is 17:2, heat up to 72°C, stir and leach for 3h, then filter , to obtain 7L filtrate A.

[0056] (2) Mix A and chloroform at a ratio of 1:0.5 by volume, stir for 3 hours, remove chlorophyll impurities, let stand to separate, and take 7L of hydroalcoholic phase B.

[0057] (3) Mix B and saturated lime water at a ratio of 1:0.1 by volume and react for 1 hour to remove tannins and other alkali-soluble impurities, and filter to obtain 8L of filtrate C.

[0058] (4) Mix C and dimethyl carbonate at a volume ratio of 1:0.3, then add 1.5 L of 10% sodium hydroxide and shake for 4 hours to remove fat-soluble impurities to obtain 9.1 L of aqueous phase D.

[0059] (5) Replace the macroporous resin D101 separation column on D for 1.5h, wash with water to remove small water-soluble molecules such as sugars, and finally elute wi...

Embodiment 3

[0062] (1) Beat 1Kg fresh sun leaves, mix according to the volume ratio of slurry to alcohol-water solution is 1:7, wherein the volume ratio of n-butanol to water is 21:2, heat up to 72°C and stir and leach for 3h After filtration, 8.2L of filtrate A was obtained.

[0063] (2) Mix A and acetone at a ratio of 1:2 by volume, stir for 3 hours, remove chlorophyll impurities, let stand to separate, and take 7.7L of hydroalcoholic phase B.

[0064] (3) Mix B and saturated lime water at a volume ratio of 1:0.5 for 3 hours to remove tannin and other alkali-soluble impurities, and filter to obtain 8.7L of filtrate C.

[0065] (4) Mix C and ethyl formate at a volume ratio of 1:1, then add 1.5 L of 10% ammonia water and shake for 4 hours to remove fat-soluble impurities, and obtain 9.1 L of aqueous phase D.

[0066] (5) Replace the macroporous resin D140 separation column on D for 1.5 hours, wash with water to remove small water-soluble molecules such as sugars, and finally elute with 2...

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Abstract

The invention discloses a method for extracting isobavachalcone from fresh angelica keiskei. The method comprises the following steps: taking fresh angelica keiskei, pulping, removing chlorophyll, removing tannin with whitewash, carrying out ester liquid-alkali liquid two-phase extraction to remove fat-soluble impurities, carrying out macroporous resin adsorption, washing with water to remove carbohydrate matters, carrying out alcohol-water gradient elution to obtain an isobavachalcone crude product, and finally carrying out secondary recrystallization to obtain an isobavachalcone fine product of which the purity is 75 percent or above. The method has the characteristics that the yield is high, the reaction time is short, the production process is pollution-free, and no side product is generated; the obtained product is simplex in composition, and high in purity, and has important application and academic values in the biological activity fields such as the antineoplastic field, the antidiabetic field, the anti-hyperlipidemia field, the hypotensive field, the antibacterial field and the anti-inflammatory field, particularly a key function in research of the pharmic structure-function relationship of chalcone.

Description

technical field [0001] The invention relates to a preparation method of isopsoralen chalcone, in particular to a method for extracting isopsoralen chalcone from fresh leaves of sun leaves. Background technique [0002] Ashitaba, also known as Longevity Grass, Longevity Vegetables, etc., is native to Izu and Hachijo Islands in Japan. It is a perennial herb of the native Celery family. Known as Ashitaba. [0003] In the Japanese works "Yamato Materia Medica" (1709) and "Revisiting the Compendium of Materia Medica Enlightenment" (1844), it is recorded that Ashitaba can strengthen the body, maintain health and prolong life. Li Shizhen, a famous doctor in my country, called Ashitaba "Binhai Angelica" as early as in "Compendium of Materia Medica" (1593), and clarified that it is sweet, pungent, warm in nature, and belongs to the liver, heart, and large intestine meridians. [0004] Domestic and foreign research in the past ten years has found that Ashitaba contains more than 10 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/835C07C45/78
CPCC07C45/78C07C49/835
Inventor 李群李子超王越吕洲刘倩倩王力平马苗刘彩虹
Owner QINGDAO UNIV
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