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Method for separating and extracting ligustilide from radices levistici

A technology for Angina radix and ligustilide, which is applied in the field of separating and extracting ligustilide from Angelica sinensis, can solve the problems of less than 98%, use, and cannot be used as a reference substance for content determination, and achieves low price, Simple steps to operate

Inactive Publication Date: 2014-08-13
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The purity of ligustilide obtained by the above method is more than 90%, but less than 98%, and cannot be used as a reference substance for content determination

Method used

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  • Method for separating and extracting ligustilide from radices levistici
  • Method for separating and extracting ligustilide from radices levistici
  • Method for separating and extracting ligustilide from radices levistici

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Grind dried Angelica sinensis produced in Gansu, weigh 100g of powder, add 0.7L of petroleum ether (60-90°C) to soak at room temperature for 2 hours, ultrasonically extract twice for 1 hour each time, filter and combine the filtrates, and concentrate the extracts under reduced pressure to obtain a paste . Then the gained paste is separated by silica gel column chromatography, adopts sherwood oil: ethyl acetate=100:1 solvent system elution, detects each fraction with thin-layer chromatography, and thin-layer chromatography condition is sherwood oil: ethyl acetate Esters = 10:1. Collect and combine the fractions containing galusene lactone, and concentrate under reduced pressure to obtain the pure product of galusene lactone. The purity is 98.15% and the yield is 0.5% as detected by high performance liquid phase.

[0020] Structural analysis of galusylactone:

[0021] Adopt nuclear magnetic resonance to carry out structural analysis to the pure product of galusene lacto...

Embodiment 2

[0030] Grind dried Angelica sinensis produced in Gansu, weigh 150g of powder, add 1.2L of petroleum ether (60-90°C) to soak at room temperature for 3 hours, ultrasonically extract 3 times, each time for 1.5 hours, filter and combine the filtrate, and concentrate the extract under reduced pressure to obtain a paste thing. Then the resulting paste is separated by silica gel column chromatography, and the solvent system elution of sherwood oil: ether=100:4 is adopted, and each fraction is detected by thin-layer chromatography, and the thin-layer chromatography condition is sherwood oil: ethyl acetate= 10:1. Collect and combine the fractions containing galusene lactone, and concentrate under reduced pressure to obtain the pure product of galusene lactone. The purity is 98.59% and the yield is 0.55% as detected by high performance liquid phase.

Embodiment 3

[0032] Grind the dried Angelica sinensis produced in Gansu, weigh 120g powder, add 1.1L petroleum ether (60-90°C) to soak at room temperature for 2.5h, ultrasonically extract 4 times, 0.5h each time, filter and combine the filtrate, and concentrate the extract under reduced pressure to obtain a paste shape. Then the resulting paste is separated by silica gel column chromatography, and the solvent system elution of sherwood oil: acetone=100:0.5 is adopted, and each fraction is detected by thin-layer chromatography, and the thin-layer chromatography condition is sherwood oil: ethyl acetate= 10:1. The fractions containing galusenide were collected and combined, and concentrated under reduced pressure to obtain pure galusenide, which was detected by high performance liquid phase with a purity of 98.23% and a yield of 0.52%.

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Abstract

The invention provides a method for separating and extracting ligustilide from radices levistici. The method comprises the following steps: by taking dry radices levistici as a raw material, soaking with petroleum ether, conducting ultrasonic extraction, filtering and concentration, separating through a silica gel column, thus obtaining high-purity ligustilide. The method is low in the price of raw materials, simple to operate, and low in environment pollution. The purity of the ligustilide obtained by adopting the method is greater than 98%, the ligustilide can be used as a chemical reference substance, and is used for quality control on angelica sinensis medical materials and preparations thereof.

Description

technical field [0001] The invention relates to a method for separating and extracting effective components of medicinal materials, in particular to a method for separating and extracting ligustilide from Angelica sinensis. technical background [0002] Ligustilide (Z-ligustilide) is the main active ingredient in traditional Chinese medicine Angelica and Chuanxiong. Its structural formula is as follows. [0003] [0004] Ligustilide has anticholinergic activities such as antispasmodic, cough and asthma. It has strong pharmacological effects on the cardiovascular and cerebrovascular system, circulatory system and immune system, and is the quality control index of angelica medicinal materials and various preparations. Existing patent has reported the preparation method of ligustilide reference substance at present, and used method is as follows: [0005] Patent CN101210003B discloses that the mixed medicine powder of angelica and chuanxiong is treated with supercritical C...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/88
CPCC07D307/88
Inventor 李震宇张争争张丽增张松秦雪梅
Owner SHANXI UNIV
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