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A kind of preparation method of Yangchuanxiongolide I

A technology of ligustilide and ligustilide, which is applied in the field of preparation of ligustilide Ⅰ, can solve the problems of limited sources, limited in-depth research and development of new drugs, complicated process, etc., and achieves the effect of increasing the content

Active Publication Date: 2019-09-20
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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Experimental program
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Effect test

Embodiment 1

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

[0028] (1) Preparation of Chuanxiong extract: 1 kg of Chuanxiong medicinal material was crushed, extracted twice with 8 times the amount of 80% ethanol, the extracts were combined, and the solvent was evaporated under reduced pressure at 45°C. The obtained extract was dispersed in water and then mixed with ethyl acetate. Ester extraction, the organic layers were combined, and the solvent was evaporated under reduced pressure at 45°C to obtain 56.4 g of an oily extract, namely 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) (with ligustilide content 19.5%, w / w; Chuanxiong lactone I 0.8%, w / w) was sequentially added to a 500 ml round-bottomed flask, and stirred at room temperature for 5 minutes; 30 g of potassium hydrogen persulfate compound salt and 12 g of sodium bicarbonate were ground and mixed, and slo...

Embodiment 2

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

[0038] (1) Preparation of Angelica sinensis extract: 5 kg of Angelica sinensis medicinal materials, crushed, passed through a No. 3 sieve, extracted by steam distillation, and obtained 27.8 g of Angelica 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) (content of ligustilide 55.1%, w / w; Yangchuanxiong lactone I 3.2%, w / w) were successively added to a 500 ml round-bottomed flask, and stirred at room temperature for 10 minutes. Take 45 g of potassium hydrogen persulfate composite salt and 16 g of sodium bicarbonate, grind and mix well, slowly add it to the reaction system, stir at room temperature for 30 minutes, then heat up to 100 ° C for 6 hours;

[0040] (3) Separation: After the reaction, the insolubles were removed by filtration, the filtrate was concentrated under reduced pressure at 50°C to remove 1,4-dioxane, ...

Embodiment 3

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

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

[0045] (2) Reaction: 200 ml of water-butanone (40:60, v / v), 10 g of ligustilide volatile oil prepared in step (1) (the content of ligustilide 28.2%, w / w; Yangchuanxiong Lactone I 1.4%, w / w) was sequentially added to a 500 ml round-bottomed 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 it to the reaction system, stir at room temperature for 30 minutes, then heat up to 60 °C for 12 hours;

[0046] (3) Separation: After the reaction, the insolubles were removed by filtration, the filtrate was concentrated under reduced pressure at 50°C to remove butano...

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Abstract

The invention discloses a preparation method of ligustilide I, which belongs to the technical field of preparation of traditional Chinese medicine components. The method uses the extract containing ligustilide as a raw material and mixes it with potassium hydrogen persulfate compound salt in an alkaline aqueous solvent After the heating reaction, the reaction solution is extracted and separated by column chromatography to obtain the pure product of ligustilide I; the extract containing ligustilide in the present invention is used as a raw material, and Ligusticum ligusticum is prepared by a method combining chemical transformation and chromatographic separation. The lactone Ⅰ has the characteristics of simple process, less solvent consumption and high yield, and is suitable for the large-scale preparation of high-purity lactone Ⅰ.

Description

technical field [0001] The invention relates to the technical field of preparation of traditional Chinese medicine ingredients, in particular to a preparation method of yangchuanxiong lactone I. Background technique [0002] Senkyunolide Ⅰ (senkyunolide Ⅰ) is a light yellow oily substance, belonging to natural phthalide compounds, mainly found in Umbelliferae, 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 yangchuanxiong lactone I is as follows: [0004] . [0005] It has been reported that Yangchuanxiong lactone I is one of the active components of traditional Chinese medicines Chuanxiong and Angelica, and it can penetrate the blood-brain barrier, reduce the pain threshold of mice with hot plate method, inhibit the writhing response caused by glacial acetic acid, and be effective in migraine hea...

Claims

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Application Information

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Patent Type & Authority Patents(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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