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High-purity polyphyllin VI preparation method and application

A high-purity technology of papaya saponin, applied in the direction of steroids, cardiovascular system diseases, organic chemistry, etc., can solve problems such as unsuitable for large-scale production, preparation of papaya saponin VI, great harm to human body, and easy volatility

Active Publication Date: 2017-07-21
YUNNAN INST OF MATERIA MEDICA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, because chloroform, methanol, and acetonitrile solvents are relatively toxic and volatile, long-term use is also relatively harmful to the human body, and the environmental pollution is also relatively serious, which limits their large-scale use in industry. Currently, they are only used in small quantities. Sample preparation of papaya saponin VI is not suitable for large-scale production and preparation of papaya saponin VI

Method used

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  • High-purity polyphyllin VI preparation method and application

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 1) After drying, the whole plant of Chonglou is coarsely crushed, extracted with 40% ethanol solution, the ratio of solid to liquid is 1:40, the number of extractions is 2 times, the extraction temperature is 90°C, and the extraction time is 60 minutes each time. The extract is filtered and the supernatant Vacuum concentration to alcohol content of 30%;

[0036] 2) The concentrated solution obtained in step 1) is centrifuged to obtain a precipitate and a supernatant, and the precipitate is discarded;

[0037] 3) Put the supernatant obtained in step 2) on a macroporous adsorption resin column D101, elute with 4 times column volume 30% ethanol and 3 times column volume 70% ethanol respectively, combine the 70% ethanol eluents, and concentrate to specific gravity If it is greater than 1.25, the extract rich in papaya saponin Ⅵ can be obtained;

[0038] 4) The sample obtained in step 3) was mixed with 100-mesh silica gel, put on a 100-mesh silica gel column, eluted with 5 ...

Embodiment 2

[0042] 1) After drying, the whole plant of Chonglou is coarsely crushed, extracted with 50% ethanol solution, the ratio of solid to liquid is 1:20, the number of extractions is 3 times, the extraction temperature is 80°C, and the extraction time is 120 minutes each time. The extract is filtered and the supernatant Adjust to 50% alcohol content for later use;

[0043] 2) The extract obtained in step 1) is centrifuged to obtain a precipitate and a supernatant, and the precipitate is discarded;

[0044] 3) The supernatant obtained in step 2) is applied to a macroporous adsorption resin column HPD-100, and eluted with 4 times column volume of 50% ethanol and 4 times column volume of 70% ethanol respectively, and the 70% ethanol eluents are combined and concentrated When the specific gravity is greater than 1.25, the extract rich in papaya saponin VI can be obtained;

[0045] 4) The sample obtained in step 3), after mixing the sample with 100 mesh silica gel, put it on a 100 mesh ...

Embodiment 3

[0049] 1) After drying, the whole plant of Chonglou is coarsely crushed, extracted with 80% ethanol solution, the ratio of solid to liquid is 1:40, the number of extractions is 4 times, the extraction temperature is 70°C, and the extraction time is 180 minutes each time. The extract is filtered and the clear liquid is vacuum Concentrate to 40% alcohol content;

[0050] 2) The concentrated solution obtained in step 1) is centrifuged to obtain a precipitate and a supernatant, and the precipitate is discarded;

[0051] 3) The supernatant obtained in step 2) is applied to a macroporous adsorption resin column HPD-700, and is eluted with 2 times column volume 50% and 3 times column volume 85% ethanol respectively, and the 85% ethanol eluents are combined and concentrated to The specific gravity is greater than 1.25, that is, the extract rich in papaya saponin Ⅵ;

[0052] 4) The sample obtained in step 3), after mixing the sample with 100 mesh silica gel, put it on a 100 mesh silic...

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Abstract

The invention relates to a high-purity polyphyllin VI preparation method and an application, and belongs to the field of Chinese herbal medicine extraction and separation. The method includes the specific steps: roughly crushing Chinese paris rhizome or wake robin medicinal materials, performing ethanol extraction; sequentially performing macroporous adsorption resin, silica gel and reverse-phase material column chromatography on extracting solution; taking ethyl acetate, ethanol and water as eluting agents and filtering, washing and drying sedimentation portions after recovering solvents by eluent to obtain high-purity polyphyllin VI. The method has the advantages that the operation steps are easily repeated, conditions are easily controlled and amplified, the solvents are low in toxicity and easy to recover, and the like. The obtained polyphyllin VI is basically free from organic solvent residues, and the purity of the polyphyllin VI reaches 98% or more. After pharmacodynamical research of the influence of mouse normal pressure hypoxia tolerance, mouse brain ischemia caused by common carotid artery ligation, rat myocardium injury caused by ischemia reperfusion, myocardial infarction caused by rat isolated heart myocardial ischemia and the like, the polyphyllin VI serving as a final product is good in effect and can be used for developing products for treating cardiovascular and cerebrovascular diseases.

Description

technical field [0001] The present invention relates to a method for extracting and preparing high-purity saponin VI from pachyphyllum pachyrhiza, trillium or other plants, and the obtained sample can be used for the treatment and prevention of ischemic cardiovascular and cerebrovascular diseases. Background technique [0002] Chonglou is a perennial herbaceous plant belonging to the family Liliaceae. There are 27 species in the world, and 25 species in my country, of which 19 species are distributed in the southwest of China. Most of them are used as medicine with rhizomes. It is a traditional Chinese medicine commonly used in my country. It is recorded that the "Pharmacopoeia of the People's Republic of China" 2015 edition contains the dried rhizomes of Paris polyphylla Smithvar.chinensis (Franch.) Hara and Paris polyphylla Smith var.yunnanensis (Franch.) Hand. Zhonglou is slightly cold in nature, bitter in taste, returns to the liver meridian, and is slightly poisonous. E...

Claims

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Application Information

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IPC IPC(8): C07J71/00A61P9/04A61P9/00
CPCC07J71/0005
Inventor 万近福李晋玉韦迪梅双喜崔涛王京昆朱兆云张梦麒丁茜郭琰
Owner YUNNAN INST OF MATERIA MEDICA
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