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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 Polygala acid and Polygala , it is difficult to simultaneously separate the two substances at one time, and the separation process needs to be repeated many times, so the time is long, the solvent consumption is large, the cost is high, the monomer yield is low, and mass production cannot be realized

Method used

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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

Examples

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Effect test

Embodiment 1

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

[0027] A, the preparation of semi-finished products: take 10 kilograms of the original medicinal material of polygala, add 80 liters of volume percentage concentration and be 70% methanol solution reflux extraction, after extracting liquid is filtered, recover methanol through decompression, add volume percentage concentration and be 30% hydrochloric acid 30 times the amount, heated and hydrolyzed at 90°C for 4 hours, then filtered out the precipitate, and the obtained precipitate was dried to obtain 200 grams of semi-finished products; The contents of acid and polygalagenin are 32% and 50% respectively.

[0028] The chromatographic condition of described analytical high performance liquid chromatograph is: chromatographic column: octadecyl bonded silica gel (4.6 * 250mm, 5 μ m); Mobile phase: tetrahydrofuran-water-...

Embodiment 2

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

[0034] A, the preparation of semi-finished products: take 10 kilograms of the original medicinal material of polygala, add 50 liters of volume percentage concentration and be 80% methanol solution reflux extraction, after extracting liquid is filtered, recover methanol through decompression, add volume percentage concentration and be 20% hydrochloric acid 20 times the amount, heated and hydrolyzed at 100°C for 2 hours, then filtered out the precipitate, and the obtained precipitate was dried to obtain 190 grams of semi-finished products; The contents of acid and polygalagenin were 34% and 52% respectively.

[0035] The chromatographic condition of described analytical high performance liquid chromatograph is: chromatographic column: octadecyl bonded silica gel (4.6 * 250mm, 5 μ m); Mobile phase: tetrahydrofuran-wate...

Embodiment 3

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

[0041] A, the preparation of semi-finished products: take 10 kilograms of the original medicinal material of polygala, add 100 liters of volume percentage concentration and be 95% methanol solution reflux extraction, after extracting liquid is filtered, recover methanol through decompression, add volume percentage concentration and be 10% hydrochloric acid 10 times the amount, heated and hydrolyzed at 80°C for 3 hours, then filtered out the precipitate, and the obtained precipitate was dried to obtain 180 grams of semi-finished products; the polygala The contents of acid and polygalagenin are 35% and 51% respectively.

[0042] The chromatographic condition of described analytical high performance liquid chromatograph is: chromatographic column: octadecyl bonded silica gel (4.6 * 250mm, 5 μ m); Mobile phase: tetrahyd...

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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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