High-speed countercurrent chromatographic method for separating terpene component in tree moss extract

A high-speed countercurrent chromatography, tree moss extract technology, applied in material separation, analysis materials, measuring devices and other directions, can solve problems such as terpene components that have not yet been seen, achieve easy popularization and use, reduce changes in properties, and process Simple process effect

Active Publication Date: 2014-11-19
CHINA TOBACCO JIANGSU INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, up to now, there are no patents and literature reports on the application of high-speed countercurrent chromatography to separate the terpene components in the extract

Method used

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  • High-speed countercurrent chromatographic method for separating terpene component in tree moss extract
  • High-speed countercurrent chromatographic method for separating terpene component in tree moss extract

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Mix n-hexane, ethyl acetate, ethanol, and water according to the volume ratio of 0.9:0.9:1:1, shake vigorously for 15 minutes, and after standing for 2 hours, the mixed solution is divided into two layers. The upper layer after layering is used as the stationary phase, and the lower layer is used as the Mobile phase: Weigh 1g of the tree moss extract sample, add 20ml of mobile phase, stir and ultrasonically disperse for 10min to obtain the sample solution to be separated.

[0034] A TBE-300 semi-preparative high-speed countercurrent chromatograph (Shanghai Tongtian Biochemical Technology Co., Ltd.) was used. The instrument was equipped with a pump, a 10-30ml sampling valve, an ultraviolet detector and a recorder. Its multilayer winding polytetrafluoroethylene tube The column capacity is about 300ml. First fill the separation column of high-speed countercurrent chromatography with stationary phase at a flow rate of 10mL / min, then turn on the speed controller to make the ...

Embodiment 2

[0038] Mix n-hexane, ethyl acetate, ethanol, and water according to the volume ratio of 0.7:0.7:0.8:1.1, shake vigorously for 20 minutes, and divide the solution into two layers after standing for 3 hours. The upper layer after layering is used as the stationary phase, and the lower layer is used as the Mobile phase: Weigh 1g of the tree moss extract sample, add 30ml of mobile phase, stir and ultrasonically disperse for 5min to obtain the sample solution to be separated.

[0039] A TBE-300 semi-preparative high-speed countercurrent chromatograph (Shanghai Tongtian Biochemical Technology Co., Ltd.) was used. The instrument was equipped with a pump, a 10-30ml sampling valve, an ultraviolet detector and a recorder. Its multilayer winding polytetrafluoroethylene tube The column capacity is about 300ml. First fill the separation column of high-speed countercurrent chromatography with a stationary phase at a flow rate of 30mL / min, then turn on the speed controller to make the high-s...

Embodiment 3

[0041] Mix n-hexane, ethyl acetate, ethanol, and water according to the volume ratio of 1.1:1.1:0.8:1.1, shake vigorously for 20 minutes, and divide the solution into two layers after standing for 2.5 hours. The upper layer after layering is used as the stationary phase, and the lower layer is As the mobile phase: Weigh 1g of the tree moss extract sample, add 25ml of the mobile phase, stir and disperse by ultrasonication for 8min to obtain the sample solution to be separated.

[0042] A TBE-300 semi-preparative high-speed countercurrent chromatograph (Shanghai Tongtian Biochemical Technology Co., Ltd.) was used. The instrument was equipped with a pump, a 10-30ml sampling valve, an ultraviolet detector and a recorder. Its multilayer winding polytetrafluoroethylene tube The column capacity is about 300ml. First fill the separation column of high-speed countercurrent chromatography with a stationary phase at a flow rate of 20mL / min, then turn on the speed controller to make the h...

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Abstract

The invention discloses a high-speed countercurrent chromatographic method for separating a terpene component in a tree moss extract. The method comprises the following steps: 1, mixing n-hexane with ethyl acetate, ethanol and water according to a volume ratio of 0.7-1.1:0.7-1.1:0.8-1.1:0.8-1.1, carrying out acute oscillation, and allowing the obtained mixture to stand in order to form two layers comprising an upper layer used as a stationary phase and a lower layer used as a mobile phase; 2, dispersing the tree moss extract by the mobile phase to obtain a sample solution to be separated; and 3, separating the sample solution through high-speed countercurrent chromatography, collecting a corresponding fraction according to an ultraviolet absorption map, and carrying out solvent removal on the obtained fraction to obtain the terpene component with the relative content of above 90%. The method has the advantages of mild conditions, high separation efficiency, good stability, simple process, and easy realization of popularization use and industrial production.

Description

technical field [0001] The invention relates to the technical field of separation methods of natural fragrance components, and more specifically relates to a method for separating terpene components from tree moss extract by applying high-speed countercurrent chromatography. Background technique [0002] Treemoss concrete is a brownish-green paste, which is made from a tea-stained lichen plant belonging to the Usneaceae genus Pleurotus genus as raw material, and extracted through petroleum ether or benzene and other certain processing techniques. have to. Treemoss extract is often used as a tobacco additive and natural fragrance raw material for daily cosmetics due to its unique natural green fragrance and strong resinous smell of liverwort. It is an important lichen spice in the international market of natural spices. [0003] The composition of extract spices is complex, and its quality and composition are not only related to plant species, but also vary with soil composi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/42
Inventor 朱怀远庄亚东秦艳华刘琪曹毅张媛尤晓娟沈晓晨刘献军
Owner CHINA TOBACCO JIANGSU INDAL
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