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Method for extracting ursolic acid from Cynomorium songaricum by using eutectic solvent/salt aqueous two-phase system

A low eutectic solvent, two-phase system technology, applied in the direction of steroids, organic chemistry, etc., to achieve the effect of short phase separation time, good biocompatibility, easy to scale up and industrial production

Active Publication Date: 2018-04-20
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no report on the use of ultrasonic-assisted deep eutectic solvent two-phase extraction combined with reverse micelles to separate ursolic acid in Cynomorium

Method used

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  • Method for extracting ursolic acid from Cynomorium songaricum by using eutectic solvent/salt aqueous two-phase system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Formation of deep eutectic solvent / salt two-phase system: K 2 HPO 4 After adding a certain amount of distilled water to fully dissolve, add a deep eutectic solvent composed of choline chloride and urea (molar ratio 1:1), and form a two-phase aqueous system after mixing. In the aqueous two-phase system, the mass percentage of the deep eutectic solvent is 25%, K 2 HPO 4 The quality score of is 38%.

[0031] (2) Ultrasonic-assisted extraction: Cynomorium powder is added to the two-phase system according to the solid-liquid ratio of 1:50 (g / g), the ultrasonic power is 300W, the pulse working mode is ultrasonic 2s, intermittent 2s, ultrasonic at 30°C Treat for 20min. Filter, and the filtrate is allowed to stand for 1h to form two phases, the upper phase is the deep eutectic solvent phase containing ursolic acid; the lower phase is the impurity-containing K 2 HPO 4 Mutually;

[0032] (3) Secondary aqueous two-phase extraction: In the above-mentioned deep eutectic s...

Embodiment 2

[0036] (1) Formation of deep eutectic solvent / salt two-phase system: K 2HPO 4 After adding a certain amount of distilled water to fully dissolve, add a deep eutectic solvent composed of choline chloride and 1.3-butanediol (molar ratio 1:2), and form an aqueous two-phase system after mixing. In the aqueous two-phase system, the mass fraction of the deep eutectic solvent is 28%, K 2 HPO 4 The mass fraction is 35%.

[0037] (2) Ultrasonic-assisted deep eutectic solvent / salt two-phase extraction: Cynomorium powder is added to the two-phase system at a solid-to-liquid ratio of 1:100 (g / g), the ultrasonic power is 500W, and the pulse working mode is Sonicate for 2s, intermittently for 2s, and sonicate at 30°C for 10min. After filtering, the filtrate was allowed to stand for 1.5 hours to form two phases, the upper phase being a deep eutectic solvent phase containing ursolic acid; the lower phase being a salt solution containing impurities.

[0038] (3) Secondary aqueous two-phas...

Embodiment 3

[0042] (1) Formation of deep eutectic solvent / salt two-phase system: K 2 HPO 4 After adding a certain amount of distilled water to fully dissolve, add a deep eutectic solvent composed of choline chloride and glycerin (molar ratio 1:1), and form a two-phase aqueous system after mixing. In the aqueous two-phase system, the mass fraction of the deep eutectic solvent is 30%, K 2 HPO 4 The quality fraction is 40%.

[0043] (2) Ultrasonic-assisted deep eutectic solvent / salt two-phase extraction: Cynomorium powder is added to the two-phase system at a solid-to-liquid ratio of 1:75 (g / g), the ultrasonic power is 350W, and the pulse working mode is Sonicate for 2s, intermittently for 2s, and sonicate at 40°C for 25min. After filtration, after the filtrate was allowed to stand for 1 h, two phases were formed, the upper phase was a deep eutectic solvent phase containing ursolic acid; the lower phase was K 2 HPO 4 solution.

[0044] (3) Secondary aqueous two-phase extraction: In th...

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Abstract

The invention provides a method for extracting ursolic acid from Cynomorium songaricum by using a eutectic solvent / salt aqueous two-phase system. The method comprises the following steps: with the eutectic solvent / salt aqueous two-phase system as an extraction solvent, subjecting the powder of Cynomorium songaricum to ultrasonic extraction at first so as to obtain a eutectic solvent phase containing ursolic acid, then carrying out pre-extraction by using a reversed micelle solution, and carrying out standing for layering, wherein an upper phase is a reversed micelle phase containing ursolic acid; and adding absolute ethyl alcohol into the reversed micelle phase containing ursolic acid for extraction, then carrying out standing and layering, wherein a lower phase is an absolute ethyl alcohol phase containing ursolic acid, and subjecting the absolute ethyl alcohol phase containing ursolic acid to pressure-reduced concentration and vacuum drying so as to obtain ursolic acid powder. According to the invention, the eutectic solvent / salt aqueous two-phase system is employed for extraction of the powder of Cynomorium songaricum, and reversed micelle extraction is employed for separation of ursolic acid in the eutectic solvent, so the method has the characteristics of short phase-splitting time, low viscosity, small possibility of emulsification and the like; the eutectic solvent and the reversed micelle solvent can be cyclically utilized; and the method is low in extraction cost, high in the purity and yield of a ursolic acid product and is a green, highly-efficient and simple separation method.

Description

technical field [0001] The invention relates to an extraction method of ursolic acid in Cynomorium, in particular to a method for extracting ursolic acid in Cynomorium by using a deep eutectic solvent / salt two-phase system, and belongs to the technical field of deep processing of natural products. Background technique [0002] Ursolic acid is a pentacyclic triterpenoid compound of α-aromatic resin, which is an important natural product in plants. It has various biological effects such as anticancer, antibacterial, antidiabetic, antiulcer, increasing immunity, and lowering blood lipids. . In recent years, ursolic acid has been paid more and more attention in the fields of food, medicine and cosmetics, and it is an important source of functional food and drug development. Cynomorium cynomorium is the dry fleshy stem of Cynomorium cynomorium, a parasitic plant of Cynomorium cylindraceae. It is mainly distributed in the northwest of my country. One of the important active ingre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
CPCC07J63/008
Inventor 张继张喜峰滕桂香
Owner NORTHWEST NORMAL UNIVERSITY
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