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Separation and preparation method of ligustilide

A technology of ligustrazolide and chuanxiong, which is applied in the field of separation and preparation of ligustrazolide, and achieves the effects of simple operation, less solvent consumption and high efficiency

Active Publication Date: 2014-08-27
CHANGSHA BROAD OCEAN BIO SCI & TECHN CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This technology does not require a solid phase carrier, and only needs to distribute the separated substance in two phases, avoiding the problems of a large number of sample adsorption, loss and pollution caused by the solid phase carrier, high sample recovery rate, simple pretreatment and posttreatment It is easy to operate. Compared with other separation methods, it does not use a solid phase carrier as a stationary phase, and can use different solvent systems and positive and negative phase elution methods to overcome sample adsorption, loss, pollution, and peak shape caused by solid phase carriers. Disadvantages such as tailing

Method used

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  • Separation and preparation method of ligustilide
  • Separation and preparation method of ligustilide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Preparation of Rhizoma Chuanxiong Extract:

[0029] Weigh Rhizoma Chuanxiong, then add 5 times the volume of ethanol, heat and reflux for extraction for 1 hour, let it stand, filter, extract the medicinal residue twice with the above method, combine the extracts, and then distill and recover the solvent under reduced pressure in a water bath to obtain Ligusticum Chuanxiong Extract The medicinal extract, the Chuanxiong extract extract is dispersed with 7 times the volume of water, and then extracted 5 times with ethyl acetate to obtain the ethyl acetate extract;

[0030] (2) separation and preparation of Ligusticolactone by high-speed countercurrent chromatography:

[0031] The two-phase solvent system uses n-hexane:ethyl acetate:ethanol:water volume ratio of 4:5:4:5. Before use, separate the upper and lower phases, and ultrasonically 20min. The upper phase of the solvent system is the stationary phase, and the lower phase is the mobile phase. Phase, pump the upper ph...

Embodiment 2

[0033] (1) Preparation of Rhizoma Chuanxiong Extract:

[0034] Weigh Rhizoma Chuanxiong, then add 12 times the volume of ethanol, heat and reflux for extraction for 3 hours, let it stand, filter, extract the medicinal residues twice again with the above method, combine the extracts, and then distill the solvent under reduced pressure in a water bath to obtain Ligusticum Chuanxiong Extract The medicinal extract, the Rhizoma Chuanxiong extract extract was dispersed with 13 times the volume of water, and then extracted 5 times with ethyl acetate to obtain the ethyl acetate extract;

[0035] (2) separation and preparation of Ligusticolactone by high-speed countercurrent chromatography:

[0036] The two-phase solvent system adopts cyclohexane:ethyl acetate:ethanol:water volume ratio of 5:6:5:6, separates the upper and lower phases before use, and ultrasonicates for 40min. The upper phase of the solvent system is used as the stationary phase, and the lower phase is For the mobile p...

Embodiment 3

[0038] (1) Preparation of Rhizoma Chuanxiong Extract

[0039] Take 1000g of Rhizoma Chuanxiong medicinal material, add 95% ethanol with 8 times the volume of medicinal material, heat and reflux for extraction for 2 hours, let it stand, and filter; use the same method to extract the medicinal residue twice, combine the extracts, and recover the solvent under reduced pressure in a water bath at 85°C. Chuanxiong extract extract was obtained; Chuanxiong extract extract was dispersed with 10 times the volume of water and extracted 5 times with ethyl acetate to obtain ethyl acetate extract as the test sample.

[0040] (2) Separation and preparation of chuanxiong lactone by high-speed countercurrent chromatography (HSCCC)

[0041] According to the results of partition coefficient determination, cyclohexane:petroleum ether:ethanol:water (4.5:5.5:4:6) was used in the two-phase solvent system, and the upper and lower phases were separated before use, and ultrasonicated for 30min. Use t...

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Abstract

The invention discloses a separation and preparation method of ligustilide. The method comprises the following steps by the technology of high-speed countercurrent chromatography. The method comprises the following steps: extracting ligusticum wallichii by a solution to obtain a ligusticum wallichii extract; extracting the ligusticum wallichii extract by ethyl acetate to obtain an ethyl acetate part; separating the ethyl acetate parts by high-speed countercurrent chromatography at the same time to obtain a plurality of ligustilide compounds which are respectively senkyunolide N, senkyunolide R, senkyunolide S and senkyunolide I through structural identification, wherein the purity is over 98%. The separation and preparation method of ligustilide disclosed by the invention has the advantages of simplicity in operation, few use level of solvent, no sample adsorption, loss and pollution, high efficiency and the like.

Description

technical field [0001] The invention relates to the technical field of extraction and separation of traditional Chinese medicines, in particular to a method for the separation and preparation of chuanxiong lactone. Background technique [0002] Chuanxiong is the rhizome of Ligusticumchuanxiong Hort., a plant of the genus Artemisia in the Umbelliferae family. It was first recorded in "Shen Nong's Materia Medica", and it is warm in nature and pungent in taste. Slightly bitter, has the effects of promoting blood circulation, dispelling wind and relieving pain; mainly treating irregular menstruation caused by blood stasis and Qi stagnation, dysmenorrhea, chest pain, headache, wind-cold-damp arthralgia, traumatic injuries caused by stagnation of liver Qi and Qi stagnation swelling and pain etc. Ligusticum chuanxiong mainly contains chemical components such as chuanxiong lactones, alkaloids and organic acids. Among them, animal experiments have proved that the main components of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/88
CPCC07D307/88
Inventor 刘向前邹亲朋戴玲潘烨
Owner CHANGSHA BROAD OCEAN BIO SCI & TECHN CO LTD
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