Method for separating and extracting apigenin, acacetin-7-O-beta-D-glucoside and apigenin-7-O-beta-D-glucoside from dendranthema indicum

A technology of Shennong chrysanthemum and glucoside, which is applied in the field of apigenin-7-O-β-D-glucoside, can solve the problems of large environmental pollution, large consumption of reagents, and low product purity, and achieve low environmental pollution and consumption The effect of less organic reagents and high product purity

Inactive Publication Date: 2010-11-24
HUBEI CHINA TOBACCO IND
View PDF0 Cites 9 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few studies on the chemical substance basis of Shennongxiangju at present. In the existing reports on the chemical components of Shennongxiangju, there is no discovery of apigenin, locustin-7-O-β-D-glucoside, celery A report on the prime-7-O-β-D-glucoside
The existing separation of apigenin, locustin-7-O-β-D-glucoside and apigenin-7-O-β-D-glucoside in Compositae phytochemical components, especially the separation of chemical components of Shennong chrysanthemum Most of the methods use repeated silica gel elution, and then use other types of expensive stationary phases and column chromatography that consumes a lot of organic reagents to separate the compounds. This method is more polluting to the environment.
For example, in the study of separation, purification and structure determination of flavonoid active ingredients in chamomile by Yang Yansong et al., apigenin-7-O-β-D-glucoside was obtained through repeated polyamide column chromatography and purification. Long cycle, large consumption of reagents, high cost and great environmental pollution
Gu Yaohua et al. used repeated silica gel column chromatography to separate apigenin and apigenin-7-O-β-D-glucoside from Boju. Great environmental pollution

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for separating and extracting apigenin, acacetin-7-O-beta-D-glucoside and apigenin-7-O-beta-D-glucoside from dendranthema indicum
  • Method for separating and extracting apigenin, acacetin-7-O-beta-D-glucoside and apigenin-7-O-beta-D-glucoside from dendranthema indicum
  • Method for separating and extracting apigenin, acacetin-7-O-beta-D-glucoside and apigenin-7-O-beta-D-glucoside from dendranthema indicum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Shennong chrysanthemum dried flowers, crushed through a 20-mesh sieve, took 3 kg, soaked in 70% ethanol for 12 hours, then extracted by percolation, collected the percolation liquid to 10 times the amount of the original medicinal material, recovered the solvent to obtain an extract, and distilled the extract with an appropriate amount of distilled water. paste suspension, sequentially extracted with petroleum ether, chloroform, and ethyl acetate to obtain three extraction parts, and then carry out normal pressure and reduced pressure 200-300 mesh silica gel column chromatography on the ethyl acetate part, and use petroleum ether-ethyl acetate, The chloroform-methanol system was repeatedly eluted, and the fractions were collected by TLC as the detection method, separated by semi-preparative high-performance liquid chromatography, concentrated, dried and recrystallized. Chromatographic conditions: mobile phase: methanol:water (63:37), flow rate: 2.5mL / min, column temperat...

Embodiment 2

[0045] Shennong chrysanthemum dried flowers, crushed through a 20-mesh sieve, took 3 kg, soaked in 70% ethanol for 12 hours, then extracted by percolation, collected the percolation liquid to 10 times the amount of the original medicinal material, recovered the solvent to obtain an extract, and distilled the extract with an appropriate amount of distilled water. Paste suspension, sequentially extracted with petroleum ether, chloroform, ethyl acetate to obtain three extraction parts, then carry out normal pressure and reduced pressure silica gel column chromatography on the ethyl acetate part, and use petroleum ether-ethyl acetate, chloroform-methanol system Repeated elution, using TLC as detection means, collected fractions, separated by semi-preparative high performance liquid chromatography, concentrated, dried and recrystallized. Chromatographic conditions: mobile phase: methanol:water (63:37), flow rate: 2.5mL / min, column temperature: 25°C, injection volume: 0.5mL.

[0046...

Embodiment 3

[0051] Shennong chrysanthemum dried flowers, crushed through a 20-mesh sieve, took 3 kg, soaked in 70% ethanol for 12 hours, then extracted by percolation, collected the percolation liquid to 10 times the amount of the original medicinal material, recovered the solvent to obtain an extract, and distilled the extract with an appropriate amount of distilled water. paste suspension, sequentially extracted with petroleum ether, chloroform, and ethyl acetate to obtain three extraction parts, and then carry out normal pressure and reduced pressure 200-300 mesh silica gel column chromatography on the ethyl acetate part, and use petroleum ether-ethyl acetate, The chloroform-methanol system was repeatedly eluted, and the fractions were collected by TLC as the detection means, separated by semi-preparative high performance liquid chromatography, the fractions were collected, concentrated, dried and recrystallized. Chromatographic conditions: mobile phase: methanol:water (63:37), flow rat...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a method for separating and extracting apigenin, acacetin-7-O-beta-D-glucoside and apigenin-7-O-beta-D-glucoside from dendranthema indicum, which belongs to a method for extracting chemical substances from a natural plant. The method is sequentially carried out according to the following steps of: 1. extract preparation; 2. extraction: sequentially extracting the extract of the dendranthema indicum by using petroleum ether, chloroform and ethyl acetate; and 3. separation and extraction: (1) carrying out normal-pressure and reduced-pressure silica column chromatography on the extracted part by using the ethyl acetate; and (2) separating fractions through a semi-preparative high-efficiency liquid chromatographic instrument to obtain the acacetin-7-O-beta-D-glucoside, the apigenin-7-O-beta-D-glucoside and the apigenin as compounds. In the method, the semi-preparative high-efficiency liquid chromatographic instrument is directly adopted for separation to obtain the three compounds after silica column chromatography is adopted, and the method has good separation effect, short time, high product purity and less environmental pollution.

Description

technical field [0001] The invention belongs to a method for extracting chemical substances from natural plants, in particular to apigenin, locustin-7-O-β-D-glucoside, apigenin-7-O- β-D-glucoside method. Background technique [0002] Shennongxiangju Dendranthema indicum (L.) Des Monl.var aromaticum Q.H.Liuet S.F.Zhang. is a new variety of Dendranthema in the family Asteraceae. It is a unique plant in Shennongjia. It is produced in Shennongjia forest area, Hubei Province, distributed at an altitude of 1200 meters Above the sunny open hillsides, roadsides, rock crevices, and open spaces beside bushes, the whole plant has a special strong aroma, and folks use its flowers and leaves dried in the shade as sachets. In the mountainous area of ​​Western Hubei, Shennong Xiangju is used to prevent and treat colds, headaches, bacillary dysentery, enteritis, constipation, coronary heart disease and high blood pressure. It can be used to extract essential oils or extracts for use in me...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/30C07D311/40C07H17/07C07H1/08B01D15/08
Inventor 卢金清李琳郭国宁
Owner HUBEI CHINA TOBACCO IND
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products