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High yield environmental protection type industrial separating method for ginseng saponin Rb1

The technology of a ginsenoside and a separation method is applied in the field of extraction and separation of effective components of traditional Chinese medicine, can solve problems such as increased production cost, high production cost, and cannot be reused, and achieves the effects of shortened production cycle, reduced production cost, and short production cycle.

Inactive Publication Date: 2005-11-09
长春三和参业科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Although in the early 1980s, the industrial production of total ginsenosides from stems and leaves of ginseng had been completed, today, only ginsenoside-Re and ginseng prepared by physical and chemical methods are among the more than 40 kinds of monomeric ginsenosides in total ginsenosides. Saponin-Rg 3 , Enzyme conversion method to produce ginsenoside-Rh 2 Three kinds of monomeric ginsenosides, such as ginsenosides, can be industrialized. Other monomeric saponins are restricted by separation technology, especially the separation process, that is, the previous solvent method and chromatography method. The process is cumbersome, inefficient, difficult to operate, and the production cost is too high. , The solvent is volatile, flammable, and toxic, posing a threat to the personal safety of production personnel and easily polluting the environment. It is limited to the preparation of a small amount of pure products in the laboratory, so it has not been able to realize factory production and industrial development.
And the traditional separation method, ginsenoside Rb 1 The yield is about 10%, and the purity can only reach about 90%. If further purification is required, only by high performance liquid chromatography
The eluent of the traditional separation method needs to be mixed with several solvents. After the production is over, the solvent recovery and separation are difficult and cannot be reused. If separation is required, production equipment needs to be added, resulting in increased production costs.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1. Column packing: take 12 kg of 200-300 mesh silica gel, add 24 liters of water-saturated n-butanol, stir while adding, remove air bubbles, soak for 10 hours, put it into a 100 cm high chromatography column, and add 36 liters of water-saturated n-butanol Alcohol elution is stable and ready for use;

[0023] 2. Separation: Take 240 grams of total ginsenosides as a sample, dissolve in a small amount of water-saturated n-butanol, add to the top of a stable chromatography column, elute with water-saturated n-butanol, and start when the color band reaches the bottom of the chromatography column Continuous sampling with a triangular flask, 50 milliliters each time, is detected by thin-layer chromatography while sampling, until no obvious spots are detected, the sampling is terminated;

[0024] 3. Recovered product: combined ginsenoside Rb 1 Part of the eluent, decompression recovery n-butanol, to obtain ginsenoside Rb 1 aqueous solution, vacuum freeze-drying, to obtain gin...

Embodiment 2

[0026] 1. Column packing: Take 12 kg of 200-300 mesh silica gel, add 24 liters of water-saturated n-butanol, stir while adding, remove air bubbles, soak for 12 hours, put it into a 100 cm high chromatography column, and add 36 liters of water-saturated n-butanol Alcohol elution is stable and ready for use;

[0027] 2. Separation: Take 300 grams of total ginsenosides as a sample, dissolve in a small amount of water-saturated n-butanol, add to the top of a stable chromatography column, and elute with water-saturated n-butanol until the color band reaches the bottom of the chromatography column. Continuous sampling with a triangular flask, 50 milliliters each time, is detected by thin-layer chromatography while sampling, until no obvious spots are detected, the sampling is terminated;

[0028] 3. Recovered product: combined ginsenoside Rb 1 Part of the eluent, decompression recovery n-butanol, to obtain ginsenoside Rb 1 aqueous solution, vacuum freeze-drying, to obtain ginsenos...

Embodiment 3

[0030] 1. Column packing: Take 12 kg of 200-300 mesh silica gel, add 24 liters of water-saturated n-butanol, stir while adding, remove air bubbles, soak for 15 hours, put it into a 100 cm high chromatography column, and add 36 liters of water-saturated n-butanol Alcohol elution is stable and ready for use;

[0031] 2. Separation: Take 400 grams of total ginsenosides as a sample, dissolve in a small amount of water-saturated n-butanol, add to the top of a stable chromatographic column, and elute with water-saturated n-butanol until the color band reaches the bottom of the chromatographic column. Continuous sampling with a triangular flask, 50 milliliters each time, is detected by thin-layer chromatography while sampling, until no obvious spots are detected, the sampling is terminated;

[0032] 3. Recovered product: combined ginsenoside Rb 1 Part of the eluent, decompression recovery n-butanol, to obtain ginsenoside Rb 1 aqueous solution, vacuum freeze-drying, to obtain ginsen...

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Abstract

The present invention relates to the extraction and separation of effective components in Chinese medicine. The ginsenoside Rb1 separating process includes dissolving ginsenoside, American ginsenoside or notoginseng general saponin in small amount of eluant, adding to stabilized chromatographic column to elute while detecting until reaching negative, merging the elutriant of ginsenoside Rb1, reducing recovering solvent, vacuum freeze drying to obtain freeze dried ginsenoside Rb1 powder, inspection and packing. The present invention has the advantages of simple technological process, short production period, no pollution, low cost, high product purity over 95 %, and high yield up to 20 %.

Description

technical field [0001] The invention belongs to a method for extracting and separating active ingredients of traditional Chinese medicines. Background technique [0002] The main bioactive components in ginseng, American ginseng and notoginseng are ginsenosides. The study of ginsenosides began in 1854, when the American scholar Garrigues obtained an amorphous substance from American ginseng produced in Canada, and named it Panaqnilon. 1 , -Rb 2 , -Rc, -Rd and -Re. In 1985, domestic scholar Wei Junxian and others isolated ginsenosides -Ro and -Rb from American ginseng 1 , -Rg 1 , -Re and pseudo-ginsenoside-F11 and other five kinds of ginsenosides. Since the 1990s, on the basis of research at home and abroad, Chinese scholars have further isolated and identified the saponins in ginseng roots and their aerial parts. Analytical methods were systematically studied, and 10 new saponins were obtained from ginseng stems and leaves. So far, more than 40 species of ginsenosides...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J9/00C07J17/00
Inventor 魏春雁李向高王秀全王德清王光学
Owner 长春三和参业科技有限公司
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