Method for preparing ligustilide

A technology of ligustilide and angelica, applied in the field of extraction and preparation of ligustilide, which can solve the problems of complex process and low purity of ligustilide

Inactive Publication Date: 2012-06-20
SHANGHAI INST OF PHARMA IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a kind of preparation method of ligustilide, which solves the technical problems of complex extraction and low purity in the extraction and preparation of ligustilide in the prior art

Method used

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  • Method for preparing ligustilide
  • Method for preparing ligustilide
  • Method for preparing ligustilide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The invention compares the effects of different ratios of angelica and chuanxiong and different supercritical extraction conditions on the extraction rate of ligustilide.

[0023] First, the effects of different ratios of angelica and chuanxiong on the extraction rate of ligustilide were compared. Compared the extraction rate of ligustilide when the mixing ratio of Angelica and Chuanxiong is 5:1~0.2:1, the experiment shows that the mixing ratio of Angelica and Chuanxiong is 0.2:1~ When 1:1, the extraction rate of ligustilide is greater than that of angelica and Chuanxiong when the mixing ratio is 1:1; when the mixing ratio of angelica and Chuanxiong is 0.33:1, the extraction rate of ligustilide highest rate. Experimental data such as figure 1 , Table 1 shows.

[0024] Table 1 Effect of different proportions of angelica and chuanxiong on the content of ligustilide

[0025]

Embodiment 2

[0027] The present invention compares the influence of different supercritical extraction conditions on the extraction rate of ligustilide. Orthogonal experiments were used to investigate the extraction temperature, extraction pressure, CO 2 The influence of four factors of flow rate and extraction time on the extraction rate of ligustilide, the experiment shows that the optimal conditions for supercritical extraction of ligustilide are: extraction temperature is 50°C, extraction pressure is 30MPa, CO 2 The flow rate is 30L / h, and the extraction time is 2.0h. The experimental data are shown in Table 2.

[0028] Table 2 Effect of different supercritical extraction conditions on the content of ligustilide

[0029]

[0030]

[0031] The mixing ratio of Angelica sinensis and Rhizoma Chuanxiong adopted in the present invention is 0.2:1~1:1 and the extraction rate of the ligustilide extracted under supercritical extraction conditions is higher than that of the prior art, and...

Embodiment 3

[0033] Put 200 g of the mixed medicinal material (0.33:1) powder (40 mesh) of Angelica sinensis and Rhizoma Chuanxiong into a 1L extraction kettle, and use supercritical CO 2 Do the extraction. The temperature of the extraction tank is 50°C and the pressure is 30MPa; the temperature of the separation tank I is 50°C and the pressure is 8MPa; the temperature of the separation tank II is 30°C and the pressure is 6MPa; 2 The flow rate is 30L / h; the extraction time is 2.0h. An extract rich in ligustilide was obtained, and the extraction rate of ligustilide was 3.23%.

[0034] Put the above extract on a medium-pressure silica gel column, and elute with petroleum ether (30-60°C)-diethyl ether (99:1) at a low temperature of 10°C and in the dark, and collect 250ml as a fraction, which is analyzed by TLC. After thin-layer chromatography inspection, HPLC determination, combined pure fractions, recovered solvent under reduced pressure at 30°C, transferred to a small bottle with ether, e...

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Abstract

The invention discloses a method for preparing ligustilide, which comprises the following steps of supercritical fluid extraction, purification by column chromatography and freeze drying. The invention extracts the extractive rich in ligustilide from mixing powder of medicinal materials of angelica sinensis and szechuan lovage rhizome through supercritical CO2 fluid; when the extractive is purified by column chromatography, the purification of the extractive can reach above 99 percent through one-time elution and repeat elution or gradient elution is not needed; the ligustilide with the purification above 99 percent is obtained after freeze drying. The invention combines three techniques of the supercritical fluid extraction, the purification by column chromatography and the freeze drying to rapidly prepare the ligustilide with the purification above 99 percent under the condition of low temperature.

Description

Technical field: [0001] The invention belongs to a method for extracting active ingredients from plants, in particular to a method for extracting and preparing ligustilide from powder of mixed medicinal materials of angelica and chuanxiong. Background technique: [0002] Ligustilide is the main active ingredient of volatile oil in Chinese angelica, Chuanxiong, Ligusticum, Chaxiong and other medicinal materials. Japanese Danggui and Korean Angelica also contain ligustilide. Modern pharmacological studies have shown that ligustilide has strong pharmacological effects on the cardiovascular and cerebrovascular systems, circulatory system, and immune system. Relaxing smooth muscle, lowering blood pressure, and analgesia can be used as index components for quality control of these medicinal materials and their related preparations. But ligustilide is unstable at room temperature, is sensitive to light, heat and oxygen, and is prone to oxidation, isomerization, dimerization, etc.,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/88A61K36/236A61K36/232
CPCY02P20/54
Inventor 杨义芳许玫
Owner SHANGHAI INST OF PHARMA IND CO LTD
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