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Method for separating yingzhaosu A in artabotrys hexapetalus roots by utilizing high-speed counter-current chromatography

A technology of high-speed countercurrent chromatography and medium hawk claw A, applied in the direction of organic chemistry, can solve the problems of low hawk claw A content, unfavorable large-scale production operation, serious pollution, etc. big effect

Inactive Publication Date: 2018-08-24
郭琴
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, yingjiaolin has pharmacological and clinical activities, has insecticidal and antimalarial effects, and has a strong inhibitory effect on rodent malaria. Liang Xiaotian and others used organic solvents such as alcohol, benzene, and petroleum ether to extract repeatedly. Sodium oxide was washed many times, activated carbon adsorption and two silica gel column chromatography were finally separated to obtain agarine A, but the content of agarine A obtained by these extraction methods is low, the pollution in the production process is serious, and it is not conducive to large-scale production operations

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Take 20Kg of hawk claw flower root coarse powder, add 95% ethanol for percolation, collect the percolation liquid with a volume 10 times the weight of the medicinal material, filter, recover the ethanol under reduced pressure and concentrate to dryness to obtain a brownish-yellow extract as a sample for later use .

[0020] Select n-hexane-dichloromethane-ethanol-water to separate and prepare agaricin on a semi-preparative high-speed countercurrent chromatograph GS10A. According to the volume ratio of 6:5:5:4, the above-mentioned solvent components were arranged in a separatory funnel, shaken up, and then stood to separate layers. After equilibrating for a period of time, separate the upper phase (mobile phase) and the lower phase (stationary phase), turn on the injection pump to pump the stationary phase into the maximum flow rate of the equipment and fill the countercurrent chromatographic column, and then turn on the high-speed countercurrent chromatographic host and...

Embodiment 2

[0022] Take 20Kg of Eagle Claw flower root coarse powder, add 85% ethanol for percolation, collect the percolation liquid with a volume 8 times the weight of the medicinal material, filter, recover ethanol under reduced pressure and concentrate to dryness to obtain a brownish yellow extract as a sample for later use .

[0023] Petroleum ether-tert-butyl methyl ether-acetone-water was selected for separation on a semi-preparative high-speed countercurrent chromatograph GS10A to prepare agaricin. According to the volume ratio of 4:3:6:2, the above-mentioned solvent components were arranged in a separatory funnel, shaken up and left to stand for stratification. After equilibrating for a period of time, separate the upper phase (mobile phase) and the lower phase (stationary phase), turn on the injection pump to pump the stationary phase into the maximum flow rate of the equipment and fill the countercurrent chromatographic column, and then turn on the high-speed countercurrent chr...

Embodiment 3

[0025] Take 20Kg of hawk claw flower root coarse powder, add 85% ethanol for percolation, collect percolation fluid with a volume 6 times the weight of medicinal materials, filter, recover ethanol under reduced pressure and concentrate to dryness to obtain a brownish-yellow extract as a sample for later use .

[0026] Select n-heptane-ether-n-butanol-water to separate and prepare agaricin on a semi-preparative high-speed countercurrent chromatograph EMC-500A. According to the volume ratio of 6:3:5:2, the above-mentioned solvent components were arranged in a separatory funnel, shaken up and allowed to stand to separate layers. After equilibrating for a period of time, separate the upper phase (mobile phase) and the lower phase (stationary phase), turn on the injection pump to pump the stationary phase into the maximum flow rate of the equipment and fill the countercurrent chromatographic column, and then turn on the high-speed countercurrent chromatographic host and The detect...

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PUM

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Abstract

The invention discloses a method for separating yingzhaosu A in artabotrys hexapetalus roots by utilizing high-speed counter-current chromatography. The method comprises the following steps: (1) percolating and extracting raw materials at room temperature; (2) carrying out high-speed counter-current chromatographic separation; (3) washing with an organic solvent; (4) carrying out alkali liquid reaction; (5) crystallizing. According to the method disclosed by the invention, percolation and extraction are adopted so that the extracting rate of the yingzhaosu A can be greatly improved; the adopted high-speed counter-current chromatographic separation has the advantages of rapid speed, less loss and high purity and the crystallization purity can be improved after washing treatment is carried out through the organic solvent.

Description

technical field [0001] The invention relates to a method for extracting and separating ahawkalin, in particular to a method for separating ahawkalin from flower roots of agaricula by using high-speed countercurrent chromatography. Background technique [0002] Eagle's Claw is Artabotrys hexapetalus (L.f.) Bhandari plant of Annonaceae, also known as Eagle's Claw, Warbler's Claw, mostly cultivated, a few are wild, mainly distributed in Zhejiang, Fujian, Jiangxi, Guangdong and other southern provinces. The root of Eagle Claw is bitter and cold in nature, and it is used in the folk to treat malaria. The components in Eagle's Claw are relatively complex. The main active ingredients in Eagle's Claw root are sesquiterpene derivatives such as A. and A. Phenicol. The seeds have been isolated to obtain Phytophyllin A and Phytophyllol A. Two kinds of flavonoid glycosides, hawkaloside A and hawkaloside B, have been isolated from the leaves of hawk's claw. Among them, yingjiaolin has p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D319/02
CPCC07D319/02
Inventor 郭琴
Owner 郭琴