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Separation preparation method of thujene, thujopsene and alpha-cedrol

A technology of thujadenene and thujene, applied in chemical instruments and methods, preparation of organic compounds, separation/purification of hydroxyl compounds, etc., to achieve the effect of overcoming irreversible adsorption, large separation amount, and peak resolution

Inactive Publication Date: 2018-11-23
郭琴
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The present invention mainly extracts essential oil compounds from thuja leaves, wherein tagodene and α-cedrol have obvious antibacterial effects, but there are few reports about the preparation and separation of high-speed countercurrent chromatography

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] The solvent system of n-hexane-ethyl acetate-methanol (5:2:3, v / v) was selected, and the volatile oil sample of Thuja thuja obtained by steam distillation was separated and prepared by semi-preparative high-speed countercurrent chromatography TBE-300A ene, thudene, and α-cedrol. The solvent components according to the above proportions were arranged in a separatory funnel, shaken up and allowed to stand for stratification. After equilibrating for a period of time, the upper phase (stationary phase) and the lower phase (mobile phase) were separated, and a semi-preparative high-speed countercurrent chromatograph was used, equipped with a KTA purifier P-900 pump and a UV detector. Weigh 105.4 mg of crude volatile oil and dissolve it in 20 ml of mobile phase for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 830r / min, pump the mobile phase into the column at a flow rate of 1.2ml / min until a dynamic balance...

Embodiment 2

[0012] The n-hexane-ethyl acetate-ethanol (5:2.5:4, v / v) solvent system was selected, and the thuja volatile oil sample obtained by steam distillation was separated and prepared by analytical high-speed countercurrent chromatography GS20 to prepare thuja and luohan Perene and alpha-cedrol. The solvent components according to the above proportions were arranged in a separatory funnel, shaken up and allowed to stand for stratification. After equilibrating for a period of time, the upper phase (stationary phase) and the lower phase (mobile phase) were separated, and a semi-preparative high-speed countercurrent chromatograph was used, equipped with an NS-1007 pump and a UV detector. Weigh 30.2 mg of crude volatile oil and dissolve it in 6 ml of mobile phase for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 850r / min, pump the mobile phase into the column at a flow rate of 0.5ml / min until a dynamic equilibrium is ...

Embodiment 3

[0014] The n-hexane-n-butanol-ethanol (5:3:2, v / v) solvent system was selected, and the thuja volatile oil sample obtained by steam distillation was separated by a semi-preparative high-speed countercurrent chromatography GS10A to prepare thujene, Thumbene and alpha-cedrol. The solvent components according to the above proportions were arranged in a separatory funnel, shaken up and allowed to stand for stratification. After equilibrating for a period of time, the upper phase (stationary phase) and the lower phase (mobile phase) were separated, and a semi-preparative high-speed countercurrent chromatograph was used, equipped with an NS-1007 pump and a UV detector. Weigh 114.5 mg of crude volatile oil and dissolve it in 15 ml of mobile phase for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 1000r / min, pump the mobile phase into the column at a flow rate of 1.0ml / min until a dynamic balance is established, inje...

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Abstract

The invention discloses a method for separating and preparing high-purity monomers including thujene, thujopsene and alpha-cedrol from thuja sutchuenensis based on a high-speed countercurrent extraction method. The method takes thuja sutchuenensis leaves as raw materials; a volatile oil sample is obtained through a water steam distillation method and is separated and purified by adopting a high-speed countercurrent chromatography extraction method to obtain the monomers including the thujene, the thujopsene and the alpha-cedrol; a solvent system is composed of n-alkanes, ethyl acetate or n-butyl alcohol and methanol or ethanol. According to the method, the purity of the obtained thujene, thujopsene and alpha-cedrol reaches 93 percent, 97 percent and 96 percent or more respectively. The method has strong controllability, good separation effect and high purity and has a large-scale preparation prospect.

Description

technical field [0001] The invention relates to a method for separating and preparing high-purity thujene, thujene and α-cedrol from thuja leaves based on high-speed countercurrent chromatography. Background technique [0002] Thuja ( Thuja sutchuenensis ) is an evergreen tree of the family Cupressaceae Thuja, a rare and endangered plant endemic to my country. This species was first discovered by French missionaries in 1892. It was once considered to be one of the three extinct Chinese endemic plants. It was rediscovered in 1999. It is distributed in the Daba Mountain Nature Reserve and the Chengkou County in the northeast of Chongqing City. Xuebaoshan Nature Reserve in Kaixian County, Hua'eshan Nature Reserve in Wanyuan City, Sichuan Province, and Wudaoxia Nature Reserve in Baokang County, Hubei Province (also found in Tianshui, Gansu). "Compendium of Materia Medica" introduces that cypress has extremely high pharmacological value: "Cypress has a long-lasting and long-las...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/14C07C13/547C07C7/04C07C7/12C07C35/37C07C29/80C07C29/76
CPCA61K36/14A61K2236/331A61K2236/53C07C7/04C07C7/12C07C29/76C07C29/80C07C2603/66C07C2603/96C07C13/547C07C35/37
Inventor 郭琴
Owner 郭琴