Method of extracting and separating costunolide and dehydrocostuslactone

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. [...

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 also relatively complicated, and the toxicity Larger organic solvents such as methanol are not recommended

[0006] Aifeng Li et al. used petroleum ether-methanol-water (5:6.5:3.5) as a solvent system to separate and obtain dehydrocosylide and cosylide with a purity of more than 98%, which is a ternary solvent The system is simpler than the quaternary system. However, the solvent used in this method contains methanol, and the separation time is extremely long. More than 250 minutes, methanol is carcinogenic and has optic nerve toxicity, which is harmful to the health of operators. The amount of solvent used for a long time Many; the retention rate of the stationary phase is low, only 50%. The higher the retention rate of the stationary phase, the more samples are loaded. 50% (Aifeng Li, et. Preparative isolation and purification of costunolide and dehydrocostuslactone from Aucklandia lappa Decne by high-speed counter-current chromatography. J. Chromatogr. A 1076, 2005, 193-197)

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