Method for indirectly measuring ligustilide content in traditional Chinese medicinal materials or Chinese patent medicines by chemical conversion method

A technology for the chemical conversion of ligustilide, applied in the field of content determination of ligustilide, can solve the problems of many reaction sites, not being used, and ligustilide not being well resolved

Active Publication Date: 2020-10-20
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Because ligustilide has a highly unsaturated conjugated system with 3 ethylenic bonds and 1 carbonyl double bond, but does not form a stable conjugated system with an aromatic ring, it has many reaction sites, strong reactivity, and relatively low free energy. Low, so Diels-Alder reactions of 1,2, 1,4 and 1,6 are easy to occur to form complex dimerization or trimerization compounds
Due to the instability of the natural chemical structure of this compound, the quality of the national pharmacopoeia standard product of ligustilide has not been well resolved, resulting in the technical problem of using ligustilide as a quantitative detection index ha

Method used

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  • Method for indirectly measuring ligustilide content in traditional Chinese medicinal materials or Chinese patent medicines by chemical conversion method
  • Method for indirectly measuring ligustilide content in traditional Chinese medicinal materials or Chinese patent medicines by chemical conversion method
  • Method for indirectly measuring ligustilide content in traditional Chinese medicinal materials or Chinese patent medicines by chemical conversion method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Example 1: Determination of the content of ligustilide in Angelica medicinal materials from different cultivation places

[0058] (1) Collection of samples of medicinal materials from the origin of Angelica sinensis: The samples of medicinal materials from the origin of Angelica sinensis measured in the patent of this invention were collected in different areas of Gansu Province and Qinghai Province during November-December 2019 (the harvesting season of Angelica sinensis), Mainly including Minxian, Zhangxian, Weiyuan, Dangchang, Zhuoni, Lintan, Minle, Tianzhu, Yongdeng counties in Gansu, Minhe, Ledu, Heping, Huzhu, Menyuan, Datong and other counties in Qinghai Province . During the collection, 6 Angelica sinensis herbs of different sizes were randomly sampled, and the names of the place of origin and the contact information of the sample donors were accurately recorded. See Table 1 for the sample information of the place of origin. After the samples were collected, th...

Embodiment 2

[0065] Embodiment 2: the content of ligustilide in Chinese patent medicine

[0066] Accurately weigh 0.5 g of Angelica sinensis (commodity in pharmacy), Chuanxiong (commodity in pharmacy), concentrated Danggui pills, Danggui tablets, Chuanxiong Chadiao pills and Suxiao Jiuxin pill powder after passing the No. Add 30 mL of methanol, weigh it, and ultrasonically treat it at 100 Hz at 40°C for 30 min. After cooling, weigh again to make up for the weight lost due to solvent volatilization during the ultrasonic process. Shake the stoppered Erlenmeyer flask. Evenly, filter with a funnel to obtain ligustilide extract. Precisely draw 1 mL of ligustilide extract, add 0.6 mL of cyclopropylamine, stir at room temperature for 1.5 h, stop the reaction, and the reaction solution is directly used as the test solution. Draw 20 μL each of the test solution and the ligustilide stock solution for sample injection, measure the content of ligustilide in the test solution by the external standard ...

Embodiment 3

[0069] Embodiment 3: Determination of the content of ligustilide in commercial angelica medicinal material

[0070] (1) Collection of specimens of Angelica sinensis: Commercialized specimens of Angelica sinensis were randomly sampled and purchased in June 2020 from Danggui City, Minxian County, Gansu Province and Huichuan Medicine Market, Weiyuan County, Gansu Province (the origin is unknown), and the staff who provided the medicine said that it was the medicine of that year (storage period of 6 to 7 months), a total of 36 samples of Angelica medicinal materials;

[0071] (2) Preparation of reference substance stock solution: Accurately weigh 0.0050 g of Ligusticum pratense reference substance, and dilute methanol to a 50 mL volumetric flask as the reference substance stock solution;

[0072] (3) Preparation of the test solution: Take an appropriate amount of commercial Angelica sinensis, pulverize it with a pulverizer and pass it through a No. 4 pharmacopoeia sieve, accuratel...

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Abstract

The invention discloses a method for indirectly measuring the accurate content of ligustilide in traditional Chinese medicinal materials or Chinese patent medicines by a chemical conversion method. The method comprises the steps of extracting and/or converting ligustilide in traditional Chinese medicinal materials or Chinese patent medicine powder; converting ligustilide with an unstable chemicalstructure in traditional Chinese medicinal materials or Chinese patent medicines into cyclopropylligustilide with a stable structure, directly measuring the content of cyclopropylligustilide through an HPLC external standard method, and then indirectly calculating the content of ligustilide in traditional Chinese medicinal materials or Chinese patent medicines through equimolar weight. The methodis used for quantitatively detecting the ligustilide content in medicines, the result is reliable, the accuracy is high, the stability and reproducibility of the method are good, and the direct targetof effectively controlling the medicine quality is achieved through application of the method.

Description

technical field [0001] The invention relates to a method for determining the content of ligustilide in Chinese medicinal materials or Chinese patent medicines, in particular to a method for indirectly calculating the accurate content of ligustilide in medicinal materials or medicines by measuring the content of ligustilide through chemical transformation, It belongs to the field of drug analysis. Background technique [0002] In the Umbelliferae plants, the plants of the genus Angelica and Ligusticum all contain phthalide compounds, such as Angelica and Rhizoma Chuanxiong and other medicinal plants. These compounds are the main components of plant volatile oils, and most of them have a strong aromatic smell. Has a rich content. These compounds have many structural types, and are generally chemically unstable, and they are easily oxidized or degraded by light, heat, and enzymes in the environment when they exist alone. However, such compounds generally have good pharmacolog...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88G01N2030/027G01N2030/047G01N2030/067G01N2030/884
Inventor 柳军玺伍鹏程
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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