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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 improved separation efficiency, mild separation environment, and large separation volume

Active Publication Date: 2011-05-25
NAT ENG RES CENT FOR TRADITIONAL CHINESE MEDICINE +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] 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

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  • 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
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Effect test

Embodiment 1

[0036] The agarwood is crushed into coarse powder, 100 g of coarse powder is added to 1000 mL of 95% ethanol, and extracted under reflux for 3 hours, 3 hours each time, filtered, and rotary evaporated to dryness to obtain a brown-black extract for later use.

[0037] Select n-heptane-chloroform-methanol-water from the solvent system on a semi-preparative high-speed countercurrent chromatograph to separate and prepare agarwood tetraol and 4'-methoxy linalane tetraol. Place the above-mentioned solvent components in a separatory funnel at a volume ratio of 0.5:3.5:2.8:2.2, shake well, and stand still for layering. After equilibrating for a period of time, the upper phase (stationary phase) and the lower phase (mobile phase) are separated, and the experimental condition temperature is 20°C. Use TBE-300A high-speed countercurrent chromatograph, equipped with KTA purifier P-900 pump, UV detector, HX-1050 thermostatic circulator. Weigh 80 mg of the sample and dissolve it in 10 mL of m...

Embodiment 2

[0039] The agarwood is crushed into coarse powder, 100 g of coarse powder is added to 1000 mL of 95% ethanol, and extracted under reflux for 3 hours, 3 hours each time, filtered, and rotary evaporated to dryness to obtain a brown-black extract for later use.

[0040] Select n-hexane-chloroform-methanol-water from the solvent system to separate and prepare agarwood tetraol and 4'-methoxy agarwood tetraol on a semi-preparative high-speed countercurrent chromatograph. Place the above-mentioned solvent components in a separatory funnel at a volume ratio of 0.3:3.7:2.6:2.4, shake well, and stand still for layering. After equilibrating for a period of time, the upper phase (stationary phase) and the lower phase (mobile phase) are separated, and the experimental condition temperature is 20°C. Use TBE-300A high-speed countercurrent chromatograph, equipped with KTA purifier P-900 pump, UV detector, HX-1050 thermostatic circulator. Weigh 30 mg of the sample and dissolve it in 10 mL of mo...

Embodiment 3

[0042] The agarwood is pulverized into coarse powder, 100 g of coarse powder is added to 1000 mL of 95% ethanol, and extracted under reflux for 3 hours, 3 hours each time, filtered, and rotary evaporated to dryness to obtain a brown-black extract for later use.

[0043] Select carbon tetrachloride-chloroform-acetone-water from the solvent system to separate and prepare agarwood tetraol and 4'-methoxy agarwood tetraol on a semi-preparative high-speed countercurrent chromatograph. The above-mentioned solvent components are arranged in a separatory funnel at a volume ratio of 0.2:3.8:3.2:1.8, shake well and stand still for layering. After equilibrating for a period of time, the upper phase (stationary phase) and the lower phase (mobile phase) are separated, and the experimental condition temperature is 20°C. Use TBE-300A high-speed countercurrent chromatograph, equipped with KTA purifier P-900 pump, UV detector, HX-1050 thermostatic circulator. Weigh 150 mg of the sample and disso...

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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 invention relates to a method for separating and preparing agarwood tetraol and 4'-methoxy agarwood tetraol, in particular to a method for separating and preparing high-purity agarwood tetraol and 4'-methoxy agarwood tetraol by using high-speed countercurrent chromatography (HSCCC) Methods. technical background [0002] Aquilaria sinensis (Lour.) Aquilaria sinensis (Lour.) Gilg resin-containing wood is called domestic agarwood, earth agarwood, and agarwood. Its taste is pungent, bitter, and has a mild temperature. The effect of relieving breath and asthma is used for chest and abdomen distension and pain, stomach cold, vomiting, hiccups, kidney deficiency and qi inverse asthma. [0003] The research on the chemical composition of domestic agarwood did not start until the 1980s. Its chemical composition can be roughly divided into three categories, namely sesquiterpenoids, aromatics and 2-(2-phenylethyl) chromones, of which 2 -(2-Phenylethyl)chromones ha...

Claims

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Application Information

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Patent Type & Authority Applications(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
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