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Method for determining ligustilide in natural medicinal preparation

A technology of ligustilide and natural medicine, which is applied in the field of analytical chemistry, can solve problems such as poor stability, difficulty in long-term storage, and unchanged measurement work, and achieve the effect of good stability and low cost

Active Publication Date: 2012-12-05
SHINEWAY PHARMA GRP LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Existing methods for the determination of ligustilide need to use pure ligustilide as a reference substance. Due to the extremely poor stability of pure ligustilide, it is very easy to It isomerized into other phthalides with similar structures, so it cannot be used as a reference substance for national legal content determination to quantitatively detect ligustilide, and it often needs to be extracted and purified by itself, and it is difficult to store for a long time, which brings great difficulties to the determination work. Large unchanged, increasing the difficulty and cost of detection
At present, there is a lack of an easy-to-operate, stable, and low-cost method for the determination of ligustilide

Method used

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  • Method for determining ligustilide in natural medicinal preparation
  • Method for determining ligustilide in natural medicinal preparation
  • Method for determining ligustilide in natural medicinal preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1 Preparation of 2-(1-pentanone)-1,5-cyclohexadienecarboxylic acid reference substance

[0038] (1) Prepare acetonitrile aqueous solution containing alkali metal hydroxide:

[0039] According to the volume ratio of acetonitrile / water of 25:75, an acetonitrile aqueous solution with an acetonitrile concentration of 25% was prepared; in every 100ml: acetonitrile aqueous solution, 2g of potassium hydroxide was added.

[0040] (2) Take 5 g of angelica oil and add 80 times the volume of the above-mentioned acetonitrile aqueous solution containing alkali metal hydroxide. Stand at 30°C for 3 days, add hydrochloric acid to adjust the pH value to neutral, add an equal volume of dichloromethane for extraction, concentrate the extract under reduced pressure, put the concentrated solution on a silica gel column, and use acetone volume fractions of 10%, 20%, and 30% respectively % acetone and petroleum ether mixture for gradient elution (the boiling range of the petroleum et...

Embodiment 2

[0047] The content determination of ligustilide in embodiment 2 angelica oil soft capsules

[0048] (1) Prepare acetonitrile aqueous solution containing alkali metal hydroxide:

[0049] According to the volume ratio of acetonitrile / water of 25:75, an acetonitrile aqueous solution with an acetonitrile concentration of 25% was prepared; in every 100ml: acetonitrile aqueous solution, 2g of potassium hydroxide was added.

[0050] (2) Preparation of the test solution

[0051] (a) Weigh 0.3g of the content of Angelica oil soft capsule, add it to 20mL of the above-mentioned acetonitrile aqueous solution containing potassium hydroxide, shake it well and place it at 30°C for 1 day, add 2M hydrochloric acid to adjust the pH to neutral, add volume Acetonitrile / water solution with a ratio of 40:60 was fixed in a 50ml volumetric flask, filtered, and the filtrate was the test solution.

[0052] (b) Preparation of reference solution

[0053] Weigh the 2-(1-pentanone)-1,5-cyclohexadienecar...

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Abstract

The invention discloses a method for detecting ligustilide in a natural medicinal preparation. The method comprises the following steps: taking 2-(1-pentanone)-1,5-cyclohexadiene formic acid, namely the hydrolysis product of the ligustilide, as a reference substance, determining the content of ligustilide in the natural medicinal preparation, fully hydrolyzing the ligustilide preparation in an acetonitrile solution containing alkali metal hydroxide, determining the content of the 2-(1-pentanone)-1,5-cyclohexadiene formic acid in the sample by use of high performance liquid chromatography, and converting the content of 2-(1-pentanone)-1.5-cyclohexadiene formic acid to the content of ligustilide according to a molar ratio 1:1. The method has the advantages of good stability, low cost, and capability of determining the content of ligustilide in the natural medicinal preparation simply, conveniently and accurately.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to a method for determining ligustilide in natural medicine preparations. Background technique [0002] Ligustilide is one of the important active ingredients in traditional Chinese medicine Angelica and Chuanxiong. It is a light yellow oily liquid with a fragrance. The boiling point is 168~169°C. It is soluble in ethanol, methanol, ether, ethyl acetate, and petroleum ether. and other organic solvents, the molecular formula is C 12 h 14 o 2 , the relative molecular mass is 190.24, and its structural formula is as follows: [0003] . [0004] The chemical structure of ligustilide is an unsaturated phthalide structure, and there is an active butenyl group at the 3-position, all of which are chemically unstable factors and are prone to various isomerization reactions. [0005] At present, the content determination methods of ligustilide in natural medicine preparat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 陈浩达刘军锋杨学林黄从海高钧张纲张状年姜海
Owner SHINEWAY PHARMA GRP LTD
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