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Method for purifying panaxoside compound-K by applying macroporous resin

A technology of ginsenosides and macroporous resins, applied in the directions of organic chemistry, steroids, chemical/physical processes, etc., can solve problems such as inability to apply on a large scale, achieve process safety and environmental protection, easy operation, high yield and high purity Effect

Active Publication Date: 2010-12-22
ZHEJIANG HISUN PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The invention discloses a new method for purifying ginsenoside compound-K by using macroporous resin, which can easily and massively obtain high-purity ginsenoside compound-K, and solves the bottleneck problem that the existing technology cannot be applied on a large scale

Method used

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  • Method for purifying panaxoside compound-K by applying macroporous resin

Examples

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Embodiment 1

[0024] Take 50L of fermentation liquid [Pei Zhou, et al.CN200410018000.0, CN1570133A[P], Example 1], filter through a filter cloth to obtain 6800g of wet bacteria, cold soak in 50L of industrial ethanol and fully stir and extract for 24 hours, filter through a filter cloth Suction filtration to obtain an ethanol extract containing 62.5 g of ginsenoside compound-K. Concentrate the ethanol extract to 2.5L under reduced pressure, add 65g of activated activated carbon powder, decolorize at room temperature for 12 hours, filter with suction, collect the filtrate, add 2.5L of water to dilute to obtain the sample solution, and use D101 macroporous resin column for sample adsorption. The column volume is 4L, the adsorption capacity of ginsenoside compound-K is about 15mg / ml wet resin, and the flow rate is 1L / h. After sample loading, first elute with 12L 50% ethanol water solution to remove pigment and impurities, then elute with 6L 80% ethanol water solution to obtain the ginsenoside ...

Embodiment 2

[0026]Take 100L of fermentation broth, filter with filter cloth to get 15kg of wet cells, cold-soak in 120L of industrial ethanol and fully stir and extract for 24 hours, filter with filter cloth to obtain ethanol extract, which contains 140g of ginsenoside compound-K. Concentrate the ethanol extract to 3L under reduced pressure, add 14g of activated activated carbon powder, reflux for 0.5 hours for decolorization, filter with suction, collect the filtrate, add 1L of water to dilute to obtain the sample solution, and use HP41 macroporous resin column for sample adsorption, column volume It is 7L, the adsorption capacity of ginsenoside compound-K is about 20mg / ml wet resin, and the flow rate is 1L / h. After loading the sample, first elute with 20L of 35% aqueous methanol to remove pigment and impurities, and then elute with 8L of 75% aqueous methanol to obtain the ginsenoside compound-K component. The solvent was recovered under reduced pressure to obtain 120 g of crude ginsenos...

Embodiment 3

[0028] Take 100L of fermentation broth, filter with filter cloth to get 15kg of wet cells, cold-soak in 120L of industrial ethanol and fully stir and extract for 24 hours, filter with filter cloth to obtain ethanol extract, which contains 140g of ginsenoside compound-K. Concentrate the ethanol extract to 3L under reduced pressure, add 70g of activated activated carbon powder, decolorize at 60°C for 1 hour, filter with suction, collect the filtrate, add 1.5L of water to dilute to obtain the sample solution, and load the sample on the AB-8 macroporous resin column Adsorption, the column volume is 7L, the adsorption capacity of ginsenoside compound-K is about 20mg / ml wet resin, and the flow rate is 1.5L / h. After loading the sample, first elute with 20L 20% isopropanol aqueous solution to remove pigment and impurities, and then elute with 8L 60% isopropanol aqueous solution to obtain the ginsenoside compound-K component. The solvent was recovered under reduced pressure to obtain 1...

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Abstract

The invention relates to a method for separating and purifying a panaxoside compound-K from microorganism zymocyte by applying macroporous resin for preparing a raw medicine. The purifying yield reaches more than 72 percent, and the content of the panaxoside compound-K in a product is more than 96 percent. The method mainly comprises the following steps of: adding ethanol into zymocyte for extracting and concentrating; decoloring by active carbon and filtering; after adding water into filter liquor for diluting, leading the filter liquor to pass through a macroporous resin chromatographic column; washing by a low-concentration organic solvent aqueous solution for removing pigment and high-polarity saponin; eluting by a high-concentration organic solvent aqueous solution to obtain a panaxoside compound-K component; and finally crystallizing to obtain the panaxoside compound-K raw medicine with the content of more than 96 percent. The invention can provide a great amount of qualified raw medicine samples for the pharmaceutical development of the panaxoside compound-K.

Description

technical field [0001] The invention relates to a method for preparing ginsenoside compound-K crude drug by using a macroporous resin. The macroporous adsorption resin used can be weak polarity or low polarity resin. Background technique [0002] Ginsenoside compound-K【20-O-β-D-glucopyranosyl-20-(S)-protopanaxadiol】is a diol-type ginsenoside, but it does not exist in natural ginseng, it is the other diol-type ginsenoside in human Major degradation product in the gut. As early as 1972, Japanese scholar Yasioka and others discovered CK for the first time when they used soil bacteria to degrade the diol-type ginsenoside Rb1, Rb2 and Rc mixture to identify the true aglycon structure, and identified the structure (I.Yosooka et al.Chem . Pharm. Bull. 1972, 20(11): 2418-2421). Through nearly ten years of research, it has been found that CK has demonstrated good biological activity in many aspects, and some even surpassed the existing first-line drugs. The medicinal value of CK ha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J17/00B01D15/08
Inventor 周伟袁留生史炳照白骅
Owner ZHEJIANG HISUN PHARMA CO LTD
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