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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-artebolide and cnidone A, to achieve the effects of solvent saving, peak shape resolution, and separation environment relaxation

Active Publication Date: 2012-01-11
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] The Chuanxiong was crushed into coarse powder, 100g of coarse powder was added to 600ml of 90% (V / V) ethanol, refluxed for 3 hours, filtered, and rotary evaporated to dryness to obtain a brownish yellow extract as a sample for later use.

[0045] Select n-hexane-ethyl acetate-methanol-water from the system on a semi-preparative high-speed counter-current chromatograph to separate and prepare z-artrenolactone and cranberry lactone A. The above-mentioned solvent components are arranged in a separatory funnel in a volume ratio of 5:6:4:6, shake well, and stand still for layering. After equilibrating for a period of time, the upper phase (stationary phase) and the lower phase (mobile phase) are separated, and the experimental condition temperature is 15°C. Use TBE-300A high-speed countercurrent chromatograph, equipped with KTA purifier P-900 pump, UV detector, HX-1050 thermostatic circulator. Weigh 70mg of the sample and dissolve it in 20ml of mobile phase for later use. Be...

Embodiment 2

[0047] The angelica is crushed into coarse powder, 100 g of coarse powder is added to 600 ml of 90% (V / V) ethanol, refluxed for 3 hours, filtered, and rotary evaporated to dryness to obtain a brownish yellow extract as a sample for use.

[0048] Select n-heptane-ethyl acetate-ethanol-water from the system on a semi-preparative high-speed counter-current chromatograph to separate and prepare z-artrenolactone and cranberry lactone. The above-mentioned solvent components are arranged in a separatory funnel according to a volume ratio of 6:3:5.5:4.5, shake well and stand still for layering. After equilibrating for a period of time, the upper phase (stationary phase) and the lower phase (mobile phase) are separated, and the experimental condition temperature is 25°C. Use TBE-300A high-speed countercurrent chromatograph, equipped with KTA purifier P-900 pump, UV detector, HX-1050 thermostatic circulator. Weigh 70mg of the sample and dissolve it in 20ml of mobile phase for later use. ...

Embodiment 3

[0050] The Chuanxiong was crushed into coarse powder, 100g of coarse powder was added to 600ml of 90% (V / V) ethanol, refluxed for 3 hours, filtered, and rotary evaporated to dryness to obtain a brownish-yellow extract as a sample for use.

[0051] Select n-hexane-diethyl ether-ethanol-water from the system to separate and prepare z-artediolide and cnidium lactone A on a semi-preparative high-speed countercurrent chromatograph. The above-mentioned solvent components are arranged in a separatory funnel according to a volume ratio of 6:4:7:3, shake well and stand still for layering. After equilibrating for a period of time, the upper phase (stationary phase) and the lower phase (mobile phase) are separated, and the experimental condition temperature is 30°C. Use TBE-300A high-speed countercurrent chromatograph, equipped with KTA purifier P-900 pump, UV detector, HX-1050 thermostatic circulator. Weigh 100mg of the sample and dissolve it in 20ml of mobile phase for later use. Befor...

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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 thecomponent 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 present invention relates to a method for preparing monomer lactone components, in particular to a method for preparing high-purity z-artediolide and cranberry lactone A. Background technique [0002] The traditional Chinese medicine Chuanxiong is the rhizome of Ligusticum chuanxiong Hort. of Ligusticum chuanxiong Hort. Mainly produced in Sichuan, it was planted as early as the Northern and Southern 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: Irregular menstruation caused by blood stasis and qi stagnation, dysmenorrhea, amenorrhea, liver stagnation and qi stagnation, chest pain, headache, wind-cold dampness, bruises, swelling and pain. Clinically, it is mainly used to treat cardiovascular, cerebrovascular, respiratory, urinary and gynecological diseases. [0003] The in...

Claims

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Application Information

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Patent Type & Authority Patents(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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