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Preparation method of senkyunolide I

A technology for yangchuanxiong lactone and ligustilide, which is applied in the field of preparation of yangchuanxiong lactone I, can solve the problems of limited sources, limited in-depth research, new drug development, complicated process and the like, and achieves the effect of increasing the content

Active Publication Date: 2018-01-23
SICHUAN ACAD OF CHINESE MEDICINE SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] For example, Chinese patent CN200910200693.8 discloses a method for preparing chuanxiong lactone I from angelica extract, using angelica medicinal material as raw material, followed by macroporous adsorption resin column chromatography, solvent extraction, silica gel column chromatography, etc. Separation technology, the steps are cumbersome, the consumption of organic solvent is large, and the final yield is only 0.07%~0.09%
[0009] Chinese patent CN 104003963 A uses high-speed countercurrent chromatography for preparation, and methods such as semi-preparative high-performance liquid chromatography and preparative high-performance liquid chromatography require high equipment and require a large investment
[0010] To sum up, the current large-scale preparation of chuanxionglide Ⅰ has many difficulties, such as consumption of raw materials, low yield, large consumption of reagents, complicated process, etc., which is not conducive to industrial production.
However, the limited source and difficult preparation of ligusticolactone Ⅰ limit its in-depth research and new drug development.

Method used

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  • Preparation method of senkyunolide I

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A preparation method of ligustilide I, the steps of which are:

[0028] (1) Preparation of Rhizoma Chuanxiong Extract: 1 kg of Rhizoma Chuanxiong, crushed, extracted twice with 8 times the amount of 80% ethanol under reflux, combined the extracts, evaporated the solvent under reduced pressure at 45°C, dispersed the obtained extract with ethyl acetate Ester extraction, combining the organic layers, and distilling off the solvent under reduced pressure at 45°C to obtain 56.4 g of oily extract, i.e. Chuanxiong extract;

[0029] (2) Reaction: 300 ml of water-ethanol mixed solution (50:50, v / v), 15 g of Chuanxiong extract prepared in step (1) (ligustilide content 19.5%, w / w; Chuanxiong lactone I 0.8%, w / w) was added to a 500 ml round bottom flask in sequence, and stirred for 5 minutes at room temperature; 30 g of potassium hydrogen persulfate compound salt and 12 g of sodium bicarbonate were finely ground and mixed, and slowly added to the reaction system , stirred at room ...

Embodiment 2

[0037] A preparation method of ligustilide I, the steps of which are:

[0038] (1) Preparation of angelica extract: 5 kg of angelica medicinal materials were crushed, passed through a No. 3 sieve, and extracted by steam distillation to obtain 27.8 g of volatile oil;

[0039] (2) Reaction: 200 ml of water-1,4-dioxane (50:50, v / v), 10 g of Angelica volatile oil prepared in step (1) (55.1% ligustilide content, w / w; Ligustilide I 3.2%, w / w) was added to a 500 ml round bottom flask in turn, and stirred at room temperature for 10 minutes. Take 45 g of potassium hydrogen persulfate compound salt and 16 g of sodium bicarbonate, grind and mix well, slowly add to the reaction system, stir at room temperature for 30 minutes, then raise the temperature to 100°C for 6 hours;

[0040] (3) Separation: After the reaction, remove the insoluble matter by filtration, concentrate the filtrate under reduced pressure at 50°C to remove 1,4-dioxane, and then extract with ethyl acetate (100 ml×3 tim...

Embodiment 3

[0043] A preparation method of ligustilide I, the steps of which are:

[0044] (1) Preparation of Ligusticum edulis extract: 2 kg of Ligusticum edulis medicinal materials were crushed, passed through a No. 3 sieve, and extracted by steam distillation to obtain 14.3 g of Ligusticum volatile oil;

[0045] (2) Reaction: Mix 200 ml of water-butanone (40:60, v / v), 10 g of Ligusticum volatile oil obtained in step (1) (ligustilide content 28.2%, w / w; Lactone I 1.4%, w / w) were successively added to a 500 ml round bottom flask and stirred at room temperature for 5 minutes. Take 30 g of potassium hydrogen persulfate compound salt and 12 g of sodium acetate, grind and mix well, slowly add to the reaction system, stir at room temperature for 30 minutes, then raise the temperature to 60°C for 12 hours;

[0046] (3) Separation: After the reaction, remove the insoluble matter by filtration, concentrate the filtrate under reduced pressure at 50°C to remove butanone, and then extract with eth...

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Abstract

The invention discloses a preparation method of senkyunolide I, and belongs to the technical field of traditional Chinese medicine component preparation. The preparation method is characterized in that extract containing ligustilide is taken as a raw material, and reaction liquor is subjected to extraction and column chromatography isolation to obtain a senkyunolide I pure product after the raw material and potassium hydrogen persulfate composite salt perform heating reaction in an alkaline water-containing solvent. According to the preparation method disclosed by the invention, the extract containing ligustilide is taken as the raw material, and senkyunolide I is prepared through a method combining chemical conversion and chromatographic separation. The preparation method has the characteristics of simple and convenient process, less solvent consumption and high yield, and is suitable for preparing high-purity senkyunolide I on a large scale.

Description

technical field [0001] The invention relates to the technical field of preparation of traditional Chinese medicine components, in particular to a preparation method of chuanxiong lactone I. Background technique [0002] Senkyunolide Ⅰ is a light yellow oily substance, belonging to natural phthalide compounds, mainly found in Umbelliferae plants, such as Chuanxiong ( Ligusticum chuanxiong Hort.), Angelica ( Angelica sinensis (Oliv.) Diels), Ligusticum ( Ligusticum sinense Oliv.) and other volatile oils or fat-soluble extracts. [0003] The chemical structure of Ligustilide Ⅰ is as follows: [0004] . [0005] It has been reported that chuanxionglide Ⅰ is one of the active ingredients of Chinese medicines Chuanxiong and Angelica, and can pass through the blood-brain barrier, can reduce the pain threshold of hot plate mice, inhibit the writhing reaction caused by glacial acetic acid, and has a great effect on migraine. Endogenous substances such as nitric oxide (NO),...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/88
Inventor 陈雏吴燕李彬杜蕾蕾
Owner SICHUAN ACAD OF CHINESE MEDICINE SCI
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