Unlock instant, AI-driven research and patent intelligence for your innovation.

Separation preparation method for high-purity agarotetrol and 4'-methoxy agarotetrol

A kind of methoxy agarwood tetraol, agarwood tetraol technology, applied in the direction of organic chemistry, etc., to achieve the effect of improving separation efficiency, large separation amount, and high peak shape resolution

Active Publication Date: 2013-08-21
NAT ENG RES CENT FOR TRADITIONAL CHINESE MEDICINE +1
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] Before the present invention, there is no public report that high-purity agaratetrol and 4'-methoxy agaratetrol are separated by high-speed countercurrent chromatography (HSCCC)

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
  • Separation preparation method for high-purity agarotetrol and 4'-methoxy agarotetrol
  • Separation preparation method for high-purity agarotetrol and 4'-methoxy agarotetrol
  • Separation preparation method for high-purity agarotetrol and 4'-methoxy agarotetrol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Crush agarwood into coarse powder, take 100g of coarse powder and add 1000mL of 95% ethanol, reflux for extraction for 3 hours, 3 hours each time, filter, and rotary evaporate to dryness to obtain a brown-black extract for later use.

[0039] Select n-heptane-chloroform-methanol-water from the solvent system to separate and prepare agarotetrol and 4'-methoxy agarotetrol on a semi-preparative high-speed countercurrent chromatograph. Put the above-mentioned solvent components in a separatory funnel according to the volume ratio of 0.5:3.5:2.8:2.2, shake well and let stand to separate layers. After equilibrating for a period of time, the upper phase (stationary phase) and the lower phase (mobile phase) were separated, and the experimental condition temperature was 20°C. Adopt TBE-300A high-speed countercurrent chromatograph, equipped with Purifier P-900 pump, UV detector, HX-1050 constant temperature circulator. Weigh 80 mg of the sample to be dissolved in 10 mL of mobi...

Embodiment 2

[0041] Crush agarwood into coarse powder, take 100g of coarse powder and add 1000mL of 95% ethanol, reflux for extraction for 3 hours, 3 hours each time, filter, and rotary evaporate to dryness to obtain a brown-black extract for later use.

[0042] Select n-hexane-chloroform-methanol-water from the solvent system to separate and prepare agarotetrol and 4'-methoxy agarotetrol on a semi-preparative high-speed countercurrent chromatograph. Put the above-mentioned solvent components in a separatory funnel according to the volume ratio of 0.3:3.7:2.6:2.4, shake well and let stand to separate layers. After equilibrating for a period of time, the upper phase (stationary phase) and the lower phase (mobile phase) were separated, and the experimental condition temperature was 20°C. Adopt TBE-300A high-speed countercurrent chromatograph, equipped with Purifier P-900 pump, UV detector, HX-1050 constant temperature circulator. Weigh 30 mg of the sample to be dissolved in 10 mL of mobile ...

Embodiment 3

[0044] Crush agarwood into coarse powder, add 100g of coarse powder to 1000mL of 95% ethanol, reflux for extraction for 3 hours, 3 hours each time, filter, and spin evaporate to dryness to obtain a brown-black extract for later use.

[0045] Select carbon tetrachloride-chloroform-acetone-water from the solvent system on a semi-preparative high-speed countercurrent chromatograph to separate and prepare agaratetrol and 4'-methoxy agaratetrol. The above-mentioned solvent components were arranged in a separatory funnel according to the volume ratio of 0.2:3.8:3.2:1.8, shaken evenly and allowed to stand to separate into layers. After equilibrating for a period of time, the upper phase (stationary phase) and the lower phase (mobile phase) were separated, and the experimental condition temperature was 20°C. Adopt TBE-300A high-speed countercurrent chromatograph, equipped with Purifier P-900 pump, UV detector, HX-1050 constant temperature circulator. Weigh 150 mg of sample injectio...

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 high-speed counter-current chromatography separation preparation method for high-purity agarotetrol and 4'-methoxy agarotetrol monomers. The method comprises the following steps of: preparing a crude agilawood extract serving as a sample introduction substance; preparing a two-phase solvent system of a stationary phase and a mobile phase; filling the stationary phase in a counter-current chromatograph separation column; rotating a main machine, and pumping the mobile phase into the column; introducing a sample by using a sample introduction valve; and receiving target components according to ultraviolet detection absorption peaks. The solvent system consists of four components (A, B, C and D), wherein the component A is normal paraffin, cycloparaffin or halogenated hydrocarbon; the component B is halogenated hydrocarbon; the component C is fatty alcohol or fatty ketone; and the component D is water. The upper phase is the stationary phase, and the lower phaseis the mobile phase. By the method, high-purity agarotetrol and 4'-methoxy agarotetrol can be obtained, and the purity can reach over 97 percent; and the method can ensure high-peak resolution, has high separation amount, mild separation environment and high reclamation rate of target compounds, and is simple and convenient to operate and easy to popularize and use.

Description

technical field [0001] The present invention relates to a method for separating and preparing agarotetrol and 4'-methoxy agarotetrol, in particular to a method for separating and preparing high-purity agarotetrol and 4'-methoxy agarotetrol by using high-speed countercurrent chromatography (HSCCC) Methods. technical background [0002] Agarwood is the resinous wood of Aquilaria sinensis (Lour.) Gilg, a plant of the family Daphneaceae. It is called domestic agarwood, earth agarwood, and agarwood. The effect of relieving asthma is used for distension and pain in the chest and abdomen, stomach cold, vomiting and hiccups, kidney deficiency and dyspnea. [0003] The research on the chemical components of domestic agarwood did not start until the 1980s, and its chemical components can be roughly divided into three categories, namely, sesquiterpenes, aromatic components and 2-(2-phenylethyl)chromones, of which 2 -(2-Phenylethyl)chromones have different degrees of anti-allergic eff...

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 Patents(China)
IPC IPC(8): C07D311/74
Inventor 张继全沈平孃杜晨捷刘雯郑克敏
Owner NAT ENG RES CENT FOR TRADITIONAL CHINESE MEDICINE