Highly effective separation purification method for polygalic acid and tenuigenin

A technology of polysapogenin and purification method, which is applied in the field of separation of active components of traditional Chinese medicinal materials, can solve the problems of inability to achieve mass production, large solvent consumption, low monomer yield, etc., and achieves less time consumption and improved processing capacity. , the effect of high yield

Inactive Publication Date: 2008-09-10
CHENGDU PUSH BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But at present, at home and abroad, different parts of Polygala medicinal materials are extracted separately, and then separated and purified by repeated silica gel column chromatography and other traditional methods to obtain finished products. However, the chemical structure and properties of Pol

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  • Highly effective separation purification method for polygalic acid and tenuigenin
  • Highly effective separation purification method for polygalic acid and tenuigenin
  • Highly effective separation purification method for polygalic acid and tenuigenin

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[0025] Example 1

[0026] A method for separating and purifying polygalaic acid and polygala sapogenin, which is characterized in that it is carried out according to the following process steps:

[0027] A. Preparation of semi-finished products: Take 10 kg of Polygala raw medicinal material, add 80 liters of methanol solution with a concentration of 70% by volume and reflux for extraction. After the extract is filtered and the methanol is recovered under reduced pressure, add hydrochloric acid with a concentration of 30% by volume. 30 times the amount, heated and hydrolyzed at a temperature of 90°C for 4 hours, and then filtered out the precipitate. After the obtained precipitate was dried, 200 grams of semi-finished product was obtained; the peak area normalization method was used to determine Polygalaceae by analytical high performance liquid chromatography The content of acid and Polygala sapogenin are 32% and 50% respectively.

[0028] The chromatographic conditions of the ana...

Example Embodiment

[0032] Example 2

[0033] A method for separating and purifying polygalaic acid and polygala sapogenin, which is characterized in that it is carried out according to the following process steps:

[0034] A. Preparation of semi-finished products: Take 10 kg of Polygala raw medicinal material, add 50 liters of methanol solution with a volume percentage of 80% for reflux extraction. After the extract is filtered and the methanol is recovered under reduced pressure, add hydrochloric acid with a volume percentage of 20%. 20 times the amount, heated and hydrolyzed at 100°C for 2 hours, and filtered out the precipitate. After drying the precipitate, 190 grams of semi-finished product were obtained; the peak area normalization method was used to determine Polygalaceae by an analytical high performance liquid chromatograph The content of acid and Polygala sapogenin were 34% and 52% respectively.

[0035] The chromatographic conditions of the analytical high performance liquid chromatograph...

Example Embodiment

[0039] Example 3

[0040] A method for separating and purifying polygalaic acid and polygala sapogenin, which is characterized in that it is carried out in the following process steps:

[0041] A. Preparation of semi-finished products: Take 10 kilograms of Polygala raw medicinal materials, add 100 liters of 95% methanol solution with a volume percentage concentration for reflux extraction. After the extract is filtered and the methanol is recovered under reduced pressure, add 10% volume percentage hydrochloric acid. 10 times the amount, heated and hydrolyzed at 80°C for 3 hours, and then filtered out the precipitate. After the obtained precipitate was dried, 180 grams of semi-finished product was obtained; the peak area normalization method was used to measure Polygalaceae by analytical high performance liquid chromatography The content of acid and Polygala sapogenin are 35% and 51% respectively.

[0042] The chromatographic conditions of the analytical high performance liquid chr...

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Abstract

The invention discloses a high efficiency separation and purification method for polygalacic acids and polygala root sapogenin. The method is as follows: firstly, polygala root raw medicinal materials are extracted by the backflow of methanol and hydrolyzed by hydrochloric acids so as to obtain semi-finished products, and the contents of the polygalacic acids and polygala root sapogenin are measured by the analysis mode high performance liquid chromatograph; secondly, an etrahydrofuran solvent is used to dissolve the semi-finished products, and by taking the mixed solvent of tetrahydrofuran-water-organic acid as an eluting mobile phase and utilizing a high efficiency preparation liquid chromatogram separating system, filtrates obtained during the step of dissolving the semi-finished products are eluted and separated so as to obtain purified products of polygalacic acids and polygala root sapogenin, purities of which are both more than 98 percent. The method has the advantages of big preparation quantity, high yield and good purity of products, and realizes the synchronous separation of polygalacic acids and polygala root sapogenin, thereby the method is suitable for the industrialized production; meanwhile, the invention also provides a high efficiency liquid phase chromatogram analysis method for polygalacic acids and polygala root sapogenin, which greatly improves the degree of separation of polygalacic acids and polygala root sapogenin in a liquid chromatogram.

Description

technical field [0001] The invention relates to a method for separating the active components of Chinese medicinal materials, which belongs to the technical field of medicine. Specifically, the invention relates to a method for separating and extracting high-purity polygala acid and polygala saponin from Polygala, and the method for extracting polygalaic acid and polygala saponin. High performance liquid chromatography analysis method. Background technique [0002] Polygalaceae is a commonly used Chinese herbal medicine. The 2005 edition of Chinese Pharmacopoeia recorded its source as Polygala tenuifolia Willd. or the dried root of Polygalaceae Polygalaceae plant Polygala tenuifolia Willd. The effect of reducing swelling. Polygala mainly contains chemical components such as saponins, resins, and fatty oils. Polygala saponin and polygalacic acid belong to polygala saponins and are the main active ingredients in polygala. Their structural formulas are as follows: [0003] ...

Claims

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Application Information

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IPC IPC(8): C07J63/00C07J75/00A61K36/69
Inventor 张黎董维珍王妙闻刘丁
Owner CHENGDU PUSH BIOLOGICAL TECH
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