Preparation process of coumarin glycoside in fraxinus depauperata

A coumarin glycoside and process technology, which is applied in the field of preparation of plant secondary metabolites, can solve the problems of unsystematic research on chemical components of ash anthracnose plant raw materials and its efficient extraction process, and achieve simple and standardized operation methods and high-efficiency preparation processes Cleansing without destroying the effect of purity

Inactive Publication Date: 2017-06-20
TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, so far, the research on the chemical constituents and efficient extrac

Method used

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  • Preparation process of coumarin glycoside in fraxinus depauperata
  • Preparation process of coumarin glycoside in fraxinus depauperata

Examples

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Effect test

Embodiment 1

[0025] Example 1: Efficient Preparation of Escinolactone 5-O-(4'-cis-caffeoyl)-β-D-glucoside from Ash Bark

[0026] Step 1: Take the ash bark raw material, wash it, dry it in the shade, then pulverize it, add an aqueous solution of acetone with a volume percentage concentration of 65% according to the mass ratio of 1:3, heat and extract 4 times, each time for 24 hours, and extract Filtrate, and concentrate the filtrate under reduced pressure to 6% of the volume of the extract to obtain a crude extract;

[0027] Step 2: Add water with 3 times the mass of the crude extract, stir, add ethyl acetate with 3 times the mass of the crude extract to extract twice, separate the ethyl acetate layer, add 3 times the mass of the crude extract to the remaining water layer Extract 2 times with petroleum ether, separate the petroleum ether layer, add dichloromethane with 3 times the mass of the crude extract to the remaining water layer and extract 2 times, separate the dichloromethane layer,...

Embodiment 2

[0030] Example 2: Efficient preparation of coumarin glycoside compound esculin 5-O-(4'-cis-caffeoyl)-β-D-glucoside from the leaves of A.

[0031] Step 1: Take the raw material of ash leaves, wash, dry in the shade, then pulverize, add acetone aqueous solution with a volume percentage concentration of 70% according to the mass ratio of 1:4, extract at room temperature for 3 times, each time for 72 hours, and filter the extract , the filtrate was concentrated under reduced pressure to 5% of the volume of the extract to obtain a crude extract;

[0032] Step 2: Add water with 4 times the mass of the crude extract, stir, add ethyl acetate with 4 times the mass of the crude extract to extract 3 times, separate the ethyl acetate layer, add 4 times the mass of the crude extract to the remaining water layer Petroleum ether was extracted 3 times, the petroleum ether layer was separated, dichloromethane with 4 times the mass of the crude extract was added to the remaining water layer for...

Embodiment 3

[0035] Example 3: Efficient preparation of the coumarin glycoside compound esculin 5-O-(4'-cis-caffeoyl)-β-D-glucoside from the root of the ash tree

[0036] Step 1: Take the raw material of the root of the ash tree, wash it, dry it in the shade, then crush it, add an aqueous solution of acetone with a volume percentage concentration of 75% according to the mass ratio of 1:5, and extract it twice with the aid of ultrasonic waves, each time for 3 hours. liquid filtration, and the filtrate was concentrated under reduced pressure to 8% of the volume of the extract to obtain a crude extract;

[0037]Step 2: Add water with 2 times the mass of the crude extract, stir, add ethyl acetate with 2 times the mass of the crude extract to extract 4 times, separate the ethyl acetate layer, add 2 times the mass of the crude extract to the remaining water layer Extract 4 times with petroleum ether, separate the petroleum ether layer, add dichloromethane with 2 times the weight of the crude ext...

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Abstract

The invention belongs to the field of preparation of plant secondary metabolism components and in particular relates to a coumarin glycoside type compound which is not reported in documents, namely esculetin-5-O-(4'-cis-caffeoyl)-beta-D-glucoside, and a clean and efficient preparation process thereof. The preparation process provided by the invention has the advantages of efficient and clean preparation process, simple and standard operation method, low raw material cost, no damages to product components, high purity and the like.

Description

technical field [0001] The invention belongs to the field of preparation of plant secondary metabolites, and specifically relates to a coumarin glycoside compound that has never been reported in the literature, that is, escinolide 5-O-(4'-cis-caffeoyl)-β-D -Glucoside (the English name of the compound is cichorigenin5-O-(4'-cis-caffeoyl)-β-D-glucopyranoside) and its clean and efficient preparation process. Background technique [0002] Fraxinus depauperata is a deciduous tree of the genus Fraxinus in the family Oleaceae. The height of the tree is generally about 5 meters. It is a unique plant in my country. It is distributed in my country's Hubei, Hunan, Shaanxi, and Henan's Funiu Mountains. It grows in areas with an altitude of 400 meters to 1,100 meters, and mostly grows in hillside miscellaneous forests. At present, there are few artificial introductions and cultivations. [0003] The winter buds of thin-flowered ash are densely covered with brown tomentose. The upper no...

Claims

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Application Information

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IPC IPC(8): C07H17/075C07H1/08
CPCC07H1/08C07H17/075
Inventor 司传领罗艳艳李光壁
Owner TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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