Method of extracting and separating costunolide and dehydrocostuslactone

A technology of dehydrocosmolide and cosmolide, which is applied in the production of bulk chemicals and organic chemistry, and can solve the problems of complex solvent types, cumbersome operation steps, and long separation time

Inactive Publication Date: 2015-02-04
SOUTHWEST UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are literature reports on the use of HSCCC technology, using the quaternary system solvent system of acetate/n-propanol or butanol/ethanol or methanol/water to treat the dehydrocresinolactone and cosmosin contained in woody The method of separating and purifying hydrocarbon lactones. The types of solvents in this system are relatively complicated, and the operation is not easy. Moreover, the boiling point of n-propanol is 97.1°C, and the boiling point of n-butanol is 117.7°C, which will bring woody hydrocarbon lactone and dehydrogenation In the pure product of woody lactone, it is difficult to remove, and it needs to be removed by purification operations such as freeze-drying or recrystallization, which increases expensive instruments and more cumbersome operation steps
In addition, some people use n-hexane-ethyl acetate-methanol-water (2:0.5:2:1) solvent system to separate the two components in woody fragrance. The solvent system in this method is al...

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  • Method of extracting and separating costunolide and dehydrocostuslactone

Examples

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Effect test

Embodiment 1

[0032] Embodiment 1 Extraction and separation method of the present invention

[0033] A. Preparation of solvent system: Prepare an appropriate amount of solution according to the ratio of petroleum ether-ethanol-water (5:7:3) at room temperature, shake it in a separatory funnel, and let it stand for stratification. The upper phase is used as the stationary phase, and the lower phase is used as the mobile phase. Mutually.

[0034]B. Sample preparation: take 100g of woody herbs (passed through a No. 3 sieve), add 500ml of petroleum ether, soak overnight, and ultrasonically extract for 30 minutes. Extracted twice in the same way. The extracts were combined, filtered, and the filtrate was spun to dryness to obtain 3.8 g of crude extract of Akira sinensis. Take 100mg of crude extract of Akira sinensis and add 20ml of mobile phase to fully dissolve the sample.

[0035] C. Separation of HSCCC by high-speed countercurrent chromatography: Fill the chromatographic column with the st...

Embodiment 2

[0039] Embodiment 2 Extraction separation method of the present invention

[0040] A. The preparation of the solvent system: prepare an appropriate amount of solution according to the ratio of petroleum ether-ethanol-water (5:5:2.5) at room temperature, shake it in a separatory funnel, and let it stand for stratification. The upper phase is used as the stationary phase, and the lower phase is used as the mobile phase. Mutually.

[0041] B. Sample preparation: Take 200mg of the crude extract of Akira sinensis and add 20ml of mobile phase to fully dissolve the sample.

[0042] C. Separation of HSCCC by high-speed countercurrent chromatography: Fill the chromatographic column with the stationary phase (upper phase) from the head end to the tail end, the main engine rotates forward at a speed of 900r / min, and then pump the mobile phase (lower phase) at a flow rate of 2ml / min , when the mobile phase flows out and the two-phase solvent reaches equilibrium in the column, the ret...

Embodiment 3

[0044] Embodiment 3 Extraction separation method of the present invention

[0045] A. Preparation of solvent system: Prepare an appropriate amount of solution according to the ratio of petroleum ether-ethanol-water (5:5:5) at room temperature, shake it in a separatory funnel, and let it stand for stratification. The upper phase is used as the stationary phase, and the lower phase is used as the mobile phase. Mutually.

[0046] B. Sample preparation: take 100g of woody herbs (passed through a No. 3 sieve), add 500ml of petroleum ether, soak overnight, and ultrasonically extract for 30 minutes. Extracted twice in the same way. The extracts were combined, filtered, and the filtrate was spun to dryness to obtain 3.8 g of crude extract of Akira sinensis. Take 100mg of crude extract of Akira sinensis and add 20ml of mobile phase to fully dissolve the sample.

[0047] C. Separation of HSCCC by high-speed countercurrent chromatography: Fill the chromatographic column with the stati...

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PUM

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Abstract

The invention provides a method of extracting and separating costunolide and dehydrocostuslactone. High speed countercurrent chromatography is adopted for separation. High speed countercurrent separation study is carried out on costunolide and dehydrocostuslactone in radix vladimiriae for the first time. according to the selected three-element system, quick layering can be carried out within 15 seconds, the stationary phase retention rate is high, although few solvent varieties are provided, the above two components can be effectively separated, and a high-purity target compound is obtained; and in addition, as petroleum ether and ethanol with minimal toxicity are adopted, the separation can be finished within 3 hours, the use amount of an organic solvent is little, the environment is little polluted, and influences on health of an operator are reduced.

Description

technical field [0001] The invention relates to a method for extracting and separating coynelide and dehydrocoynelide. Background technique [0002] Cinerea Ling is the dry root of Vladimiria souliei (Franch.) Ling or Vladimiria souliei (Franch.) Ling var. cinerea Ling of Compositae, which can promote Qi and relieve pain. Because Sichuan Aba Tibetan Autonomous Prefecture is one of its main production areas, it is also considered a kind of Tibetan medicinal materials and is widely used in Tibetan medicine and Tibetan medicine. [0003] There are volatile oil components in the root of Akiras chuangiana. At present, more than 20 kinds of components have been identified by GC / MS. Gua-4(15), 10(14), 11(13)-triene-12,6α-lactone [guaia-4(15), 10(14), 11(13)-triene-12,6α- olide], 3β-acetoxyguaia-4(15), 10(14), 11(13)-triene-12, 6α-lactone [3β-acetoxyguaia-4(15), 10(14) , 11(13)-trien-12,6α-olide], 3β-hydroxy-11βH-guaiac-4(15), 10(14) diene-12,6α-lactone and other components. [...

Claims

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Application Information

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IPC IPC(8): C07D307/93
CPCC07D307/93Y02P20/54
Inventor 吕露阳刘圆鲁建美张吉仲张志锋曾锐
Owner SOUTHWEST UNIVERSITY FOR NATIONALITIES
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