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Method for extraction and content determination of lignan components of Chinese magnoliavine fruit

A technology of lignans and schisandrin, which is applied in the direction of medical preparations containing active ingredients, plant/algae/fungus/moss components, material separation, etc., can solve the problem of low extraction efficiency, and achieve favorable extraction, Simple operation effect

Inactive Publication Date: 2019-10-18
HARBIN UNIV OF COMMERCE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problem of low extraction efficiency of lignans in Schisandra chinensis, the present invention provides a method for extracting and refining lignans from Schisandra chinensis, the technical scheme is as follows:

Method used

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  • Method for extraction and content determination of lignan components of Chinese magnoliavine fruit
  • Method for extraction and content determination of lignan components of Chinese magnoliavine fruit
  • Method for extraction and content determination of lignan components of Chinese magnoliavine fruit

Examples

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Effect test

Embodiment 1

[0043] Example 1. Flash extraction method for extracting lignans from Schisandra.

[0044] 1) Schisandra fruit and ethyl acetate are mixed according to the material-to-liquid ratio of 1g:(1.5-6)mL, and the flash extractor is used to extract 1-6 times under the conditions of voltage 380V and rotation speed 5000r / min, each time 30-100s , Combined extracts;

[0045] 2) After concentrating the extract obtained in step 1), remove ethyl acetate to obtain an extract;

[0046] 3) After silica gel column chromatography, gradient elution is used. The eluent used is a mixture of petroleum ether and ethyl acetate. The volume ratio of petroleum ether to ethyl acetate in the eluent is 100:1 and 50:1 respectively. , 25:1, 10:1, 3:1, 1:1, gradient elution is carried out in sequence according to the above volume ratio, the obtained fractions are concentrated, the fractions with the same composition are combined, and the fractions with fewer components are repeated by column chromatography Or recrys...

Embodiment 2

[0105] Example 2. Flash extraction method for extracting lignans from Schisandra.

[0106] This embodiment takes the best extraction parameters as an example, combined with figure 1 , Describe the extraction method of lignans in Schisandra.

[0107] 1) 4 kg of schisandra fruit was mixed with ethyl acetate according to the material-to-liquid ratio of 1g:3mL, and extracted 3 times with a flash extractor, each 60s, and the extracts were combined;

[0108] 2) After concentrating the extract obtained in step 1), remove ethyl acetate to obtain an extract;

[0109] 3) Then gradient elution after silica gel column chromatography, the eluent used is a mixture of petroleum ether and ethyl acetate, the eluent ratio is 100:1, 50:1, 25:1, 10:1, 3 :1, 1:1, gradient elution is performed in sequence according to the above volume ratio, the obtained fractions are concentrated, and the fractions with the same composition are combined. A total of 11 compounds were obtained after separation, compound 1-...

Embodiment 3

[0164] Example 3. A method for simultaneously determining the content of lignans in the schisandra extract obtained by flash extraction.

[0165] 1) 10g of schisandra fruit is mixed with ethyl acetate according to the material-liquid ratio of 1g:3mL, and extracted 3 times with a flash extractor, each time is 60s, and the extracts are combined;

[0166] 2) Then it is concentrated by a rotary evaporator to remove the residual extraction solvent to obtain 1.22 g of ethyl acetate extract;

[0167] 3) Accurately weigh 5 mg of ethyl acetate extract, dilute it in 10 mL of methanol, and store it in a refrigerator at -20°C as the test solution for use. Analyze by high performance liquid chromatography, record the peak area of ​​the components to be tested, and calculate the contents of schisandrin A, schisandrin B, schisandrin C, schisandrin A, and schisandrin B by calculating the standard curve equation of each component to be tested. . Chromatographic conditions:

[0168] Chromatographic c...

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Abstract

A method for extraction and content determination of lignan components of Chinese magnoliavine fruit belongs to the technical field of preparation of effective components of Chinese magnoliavine fruit. To solve the problem of low extraction efficiency of lignan components in Chinese magnoliavine fruit, the invention provides a method for extraction of lignan components, which comprises the following steps: 1) mixing Chinese magnoliavine fruit with ethyl acetate in a solid-to-liquid ratio of 1 g:(1.5-6) mL, carrying out extraction with a flash extractor for 1 to 6 times, 30 to 100 seconds eachtime, and putting the extracts together; 2) concentrating the extract from the step 1) and then removing ethyl acetate to obtain an extract; and 3) subjecting the extract to silica-gel column chromatography and subsequent gradient elution, thereby obtaining the lignan components of Chinese magnoliavine fruit. The invention also provides a method for simultaneous determination of lignan componentsof Chinese magnoliavine fruit by high performance liquid chromatography. The method for extraction and content determination of lignan components of Chinese magnoliavine fruit is suitable for deep processing of Chinese magnoliavine fruit.

Description

Technical field [0001] The invention belongs to the technical field of preparation of schisandra active ingredients, and specifically relates to a method for extraction and content determination of schisandra lignans. Background technique [0002] Schisandra is a plant widely recognized in traditional Chinese medicine and modern Chinese medicine. It belongs to the Magnoliaceae and is the dried and mature fruit of Schisandra. It has been a precious Chinese medicinal material since ancient times. Schisandra has the effects of replenishing qi, solidifying surface and antiperspirant, and is often used in clinical applications to treat gastrointestinal diseases, respiratory failure, cardiovascular diseases and other types of diseases. Schisandra contains a variety of chemical components, of which the total content of schisandrin lignan compounds is 2%-8%, which is the most content component, including schisandrin A, schisandrin B, schisandrin A and hundreds of chemical components . ...

Claims

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Application Information

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IPC IPC(8): C07D493/04C07D317/70C07J9/00G01N30/02G01N30/06A61K36/57A61P1/00A61P11/00A61P9/00
CPCA61K36/57A61K2236/33A61K2236/53A61P1/00A61P9/00A61P11/00C07D317/70C07D493/04C07J9/00G01N30/02G01N30/06
Inventor 胡荻魏国伟邢志华于剑平刘思怡
Owner HARBIN UNIV OF COMMERCE
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