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Method for preparing high purity z-ligustilide and cnidilide A

A technology of artebenolide and cnidone, which is applied in the field of preparation of high-purity z-artebenolide and cnidone A, and achieves the effects of peak shape resolution, solvent saving, and large separation volume

Active Publication Date: 2010-06-30
NAT ENG RES CENT FOR TRADITIONAL CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] At present, there is no report on the simultaneous preparation of high-purity z-artebolactone and cnidone A by using HSCCC

Method used

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  • Method for preparing high purity z-ligustilide and cnidilide A
  • Method for preparing high purity z-ligustilide and cnidilide A
  • Method for preparing high purity z-ligustilide and cnidilide A

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Crush Rhizoma Chuanxiong into coarse powder, take 100g of coarse powder and add 600ml of 90% (V / V) ethanol, reflux for extraction for 3 hours, filter, and rotary evaporate to dryness to obtain a brownish-yellow extract as a sample for later use.

[0045] From the system, select n-hexane-ethyl acetate-methanol-water on a semi-preparative high-speed countercurrent chromatograph to separate and prepare z-artemisinin and cnidone A. The above-mentioned solvent components were arranged in a separatory funnel according to the volume ratio of 5:6:4:6, and the mixture was left to stand and separated after shaking. After equilibrating for a period of time, the upper phase (stationary phase) and the lower phase (mobile phase) were separated, and the experimental condition temperature was 15°C. Adopt TBE-300A high-speed countercurrent chromatograph, equipped with KTA purifier P-900 pump, UV detector, HX-1050 constant temperature circulator. Weigh 70mg of sample injection and dis...

Embodiment 2

[0047] Grind Angelica sinensis into a coarse powder, add 100g of coarse powder to 600ml of 90% (V / V) ethanol, reflux for extraction for 3 hours, filter, and rotary evaporate to dryness to obtain a brownish-yellow extract as a sample for later use.

[0048] From the system, select n-heptane-ethyl acetate-ethanol-water on a semi-preparative high-speed countercurrent chromatograph to separate and prepare z-artemisinin and cnidone A. The above-mentioned solvent components were arranged in a separatory funnel according to a volume ratio of 6:3:5.5:4.5, shaken up and allowed to stand to separate into layers. After equilibrating for a period of time, the upper phase (stationary phase) and the lower phase (mobile phase) were separated, and the experimental condition temperature was 25°C. Adopt TBE-300A high-speed countercurrent chromatograph, equipped with KTA purifier P-900 pump, UV detector, HX-1050 constant temperature circulator. Weigh 70mg of sample injection and dissolve in 2...

Embodiment 3

[0050] Crush Rhizoma Chuanxiong into coarse powder, take 100g of coarse powder and add 600ml of 90% (V / V) ethanol, reflux for extraction for 3 hours, filter, and rotary evaporate to dryness to obtain a brownish-yellow extract as a sample for later use.

[0051] Select n-hexane-diethyl ether-ethanol-water from the system on a semi-preparative high-speed countercurrent chromatograph to separate and prepare z-artebenolide and cnidone A. The above-mentioned solvent components were arranged in a separatory funnel according to the volume ratio of 6:4:7:3, shaken up and left to stand for stratification. After equilibrating for a period of time, the upper phase (stationary phase) and the lower phase (mobile phase) were separated, and the experimental condition temperature was 30°C. Adopt TBE-300A high-speed countercurrent chromatograph, equipped with KTA purifier P-900 pump, UV detector, HX-1050 constant temperature circulator. Weigh 100mg of sample injection and dissolve it in 20m...

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Abstract

The invention discloses a method for preparing high purity z-ligustilide and cnidilide A, which is characterized by adopting high-speed countercurrent chromatography and comprises the following steps: preparing the crude extract of rhizoma ligustici wallichii or angelica as a sample injection substance; preparing a solvent system forming stationary phase and mobile phase; filling the stationary phase into a countercurrent chromatography column; then rotating a host machine, pumping the mobile phase into the column, or simultaneously pumping the stationary phase and the mobile phase into the column and then rotating the host machine; and injecting samples from an injection valve, receiving target components according to a map of a detector and obtaining the z-ligustilide and cnidilide A through separation. The solvent system is formed by four components (A, B, C and D). The component A is n-alkane, the component B is fatty ether, the component C is fatty alcohol or fatty ketone and the component D is water. The z-ligustilide and cnidilide A with purity higher than 95% can be obtained by the method. The method is simple and convenient, easy to operate, high in recovery and easy to promote and use.

Description

technical field [0001] The invention relates to a preparation method of a monomeric lactone component, in particular to a preparation method of high-purity z-artebenolide and cnidone A. Background technique [0002] Chuanxiong, a traditional Chinese medicine, is the rhizome of Ligusticum chuanxiong Hort., a plant of the genus Ligusticum in the Umbelliferae family. It was first recorded in "Shen Nong's Herbal Classic". It is mainly produced in Sichuan. It was planted as early as the Southern and Northern Dynasties, and now it is also planted in other provinces. It is warm in nature, pungent in taste, slightly bitter, and has the effects of promoting blood circulation, promoting qi, dispelling wind and relieving pain. Indications for irregular menstruation and amenorrhea due to blood stasis and qi stagnation, chest and hypochondrium pain caused by stagnation of liver and qi stagnation, headache, wind-cold-damp arthralgia, swelling and pain from falls and other diseases. Clin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/88A61K36/236
Inventor 刘雯张继全沈平孃阮克锋王玲玲
Owner NAT ENG RES CENT FOR TRADITIONAL CHINESE MEDICINE
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