Method of preparing four active substances such as cycloartenyl ferulate by separation

A technology of pineapple enol ferulate and sitosterol ferulate, which is applied in the field of separating and preparing four active substances of pineapple enol ferulate, and can solve problems such as the inability to obtain extremely high-purity monomers.

Inactive Publication Date: 2018-09-21
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] It is reported in existing literature that sterol ferulic acid ester is separated from rice bran by column chromatography, but the monomer wi

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Select n-hexane-acetonitrile on a semi-preparative countercurrent chromatograph GS10AB to separate and purify rice bran extract. First, the above solvent components are prepared in a separatory funnel according to a volume ratio of 1:1, shake well and then stand to separate layers. After equilibrating for a period of time, separate the upper phase and the lower phase, take the lower phase as the stationary phase, and the upper phase as the mobile phase. A semi-preparative high-speed countercurrent chromatograph is used, equipped with an NS-1007 pump, a 20mL injection valve, a polytetrafluoroethylene column with a column volume of 240mL, an 8823A-UV ultraviolet detector, and a Yokogawa3057 portable recorder. Weigh 200mg of rice bran extract and dissolve in 5mL upper phase and 5mL lower phase mixed solution for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 800rpm, and pump the mobile phase into the colum...

Embodiment 2

[0013] Select n-heptane-dichloromethane-acetonitrile on the semi-preparative countercurrent chromatograph GS10A to separate the rice bran extract. Set layers. After equilibrating for a period of time, separate the upper and lower phases, take the lower phase as the stationary phase, and the upper phase as the mobile phase. A semi-preparative high-speed countercurrent chromatograph is used, equipped with NS-1007 pump, 20mL injection valve, polytetrafluoroethylene column with a column volume of 230mL, 8823A-UV ultraviolet detector, and Yokogawa 3057 portable recorder. Weigh 128.5mg of rice bran extract and dissolve in 5mL upper phase and 5mL lower phase mixed solution for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 800rpm, and pump the mobile phase into the column at a flow rate of 2.0mL / min; after the dynamic equilibrium of the entire system is established, inject the sample through the injection valve; the...

Embodiment 3

[0015] Select n-pentane-dichloromethane-acetonitrile on the semi-preparative countercurrent chromatograph EMC-500 to separate and purify the rice bran extract. Let it stand for layering. After equilibrating for a period of time, separate the upper phase and the lower phase, take the lower phase as the stationary phase, and the upper phase as the mobile phase. A semi-preparative high-speed countercurrent chromatograph is used, equipped with NS-1007 pump, 20mL injection valve, polytetrafluoroethylene column with a column volume of 500mL, 8823A-UV ultraviolet detector, and Yokogawa 3057 portable recorder. Weigh 400.2mg of rice bran extract and dissolve in 5mL upper phase and 5mL lower phase mixed solution for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 800rpm, and pump the mobile phase into the column at a flow rate of 2.0mL / min; after the dynamic equilibrium of the entire system is established, inject the sa...

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Abstract

The invention relates to a method of preparing high-purity monomer cycloartenyl ferulate, 24-methylene cycloartenyl ferulate, campesterol ferulate and sitosterol ferulate from a rice bran extract through separation by counter-current chromatography. The four active substances such as high-purity cycloartenyl ferulate are prepared from the rice bran extract through separation by the counter-currentchromatography; a solvent systems comprises three ingredients: petroleum ether or normal paraffin, dichloromethane and acetonitrile or fatty alcohol at a volume ratio of 10:(0-3):(7-12); the method is applicable to preparation of monomer cycloartenyl ferulate, 24-methylene cycloartenyl ferulate, campesterol ferulate and sitosterol ferulate by using various models of counter-current chromatographs; many crude products or synthetic mixtures can be introduced directly; the purity of separated cycloartenyl ferulate and sitosterol ferulate reaches above 95%; and the purity of 24-methylene cycloartenyl ferulate and campesterol ferulate reaches above 90%.

Description

technical field [0001] The invention relates to a high-purity monomer cycloartenol ferulate, 24-methylenecycloartenol ferulate and campesterol arabinate separated from rice bran extract by high-speed countercurrent chromatography. Preparation and separation method of ferulic acid ester and sitosterol ferulic acid ester. Background technique [0002] Rice is the second largest crop in the world, with an annual output of about 583 million tons. my country is the largest rice producer in the world, with an annual output of more than 200 million tons of rice, and an annual output of rice bran of about 14 million tons. Rice bran is one of the valuable by-products of the rice processing industry. It has been confirmed that a large amount of bioactive components such as sterol ferulate (about 2510-6860 μg / g) are distributed in rice bran and other grain processing wastes, mainly cyclo Carpine alcohol ferulate and campesterol ferulate, of which cycloartenol ferulate accounts for 32%...

Claims

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Application Information

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IPC IPC(8): C07J53/00C07J9/00
CPCC07J9/00C07J53/004
Inventor 魏芸车芬芳
Owner BEIJING UNIV OF CHEM TECH
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