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Method for separating and purifying monomer compounds in Stenoloma chusanum(Linn.)Ching

A technology for the separation and purification of Golden Flower Grass, which is applied in the field of pharmacy, can solve the problems of complicated operation, cumbersome operation, and low separation efficiency, and achieve the effects of shortening the extraction cycle, improving production efficiency, and reducing costs

Inactive Publication Date: 2011-11-16
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, column chromatography or recrystallization methods are mostly used at home and abroad to separate and purify, but the operation is very cumbersome, and the separation efficiency is not high, and it is difficult to obtain high-purity products
For example, in the document "Research on the Chemical Components of Golden Flower Grass Flavonoids", the method disclosed in this document is to obtain the monomer components by multiple extractions with organic solvents and repeated silica gel column chromatography. The yield is low and the operation is complicated, so it is only suitable for laboratory components. Analysis and Identification
Such as the patent (publication number is: CN101972283A) "a kind of preparation method of total flavonoids of Golden Flower Grass", the method disclosed in this patent is to adopt cellulase extraction and macroporous resin adsorption to obtain total flavonoids extract, but cannot obtain single body composition

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Take Golden Flower Grass as raw material, crush it, take 1kg, add 8 times (V / W) 75% ethanol solution to soak, then ultrasonically treat for 0.5h, filter to obtain the extract, concentrate until it has no alcohol smell, and put it on D-101 Macroporous resin adsorption, first eluted with distilled water until the lower column liquid is colorless, then eluted with 8L 65% ethanol solution, collected the eluate, concentrated to extract, dissolved with lye, filtered, added acid to the filtrate to adjust pH4, filtered The precipitate was removed, washed with water until neutral, and dried to obtain the crude product; the chloroform, methanol, n-butanol, and water were prepared in a volume ratio of 8:9:2:8, placed in a separatory funnel, fully shaken, left to stand, and separated into layers , the upper phase is the stationary phase, the lower phase is the mobile phase, and the injection valve is in the sampling state. The stationary phase is filled with the chromatographic sepa...

Embodiment 2

[0018] Take Golden Flower Grass as raw material, crush it, take 1kg, add 10 times (V / W) 75% ethanol solution to soak, microwave for 0.5h, filter to get the extract, concentrate until it has no alcohol smell, and put it on X-5 Macroporous resin adsorption, first elute with distilled water until the lower column liquid is colorless, then elute with 6L 50% ethanol solution, collect the eluate, concentrate to extract, add lye to dissolve, filter, add acid to the filtrate to adjust pH2, filter The precipitate was removed, washed with water until neutral, and dried to obtain the crude product; the chloroform, methanol, n-butanol, and water were prepared in a volume ratio of 10:9:1:6, placed in a separatory funnel, shaken fully, left to stand, and separated into layers , the upper phase is the stationary phase, the lower phase is the mobile phase, and the injection valve is in the sampling state. The stationary phase is filled with the chromatographic separation column of the counterc...

Embodiment 3

[0020] Take Golden Flower Grass as raw material, crush it, take 2kg, add 12 times (V / W) 75% ethanol solution to soak, microwave treatment for 0.6h, filter to obtain the extract, concentrate until it has no alcohol smell, and put it on LSA-21 Macroporous resin adsorption, first elute with distilled water until the lower column liquid is colorless, then elute with 15L of 70% ethanol solution, collect the eluate, concentrate to extract, add alkali solution to dissolve, filter, add acid to the filtrate to adjust pH3, filter The precipitate was removed, washed with water until neutral, and dried to obtain the crude product; the chloroform, methanol, n-butanol, and water were prepared in a volume ratio of 10:10:1:6, placed in a separatory funnel, fully shaken, left to stand, and separated , the upper phase is the stationary phase, the lower phase is the mobile phase, and the injection valve is in the sampling state. The stationary phase is filled with the chromatographic separation c...

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Abstract

The invention relates to a method for separating and purifying monomer compounds in Stenoloma chusanum(Linn.)Ching, which comprises the following steps of: soaking the Stenoloma chusanum(Linn.)Ching serving as a raw material in an alcoholic solution, performing ultrasonic or microwave treating to obtain an extracting solution, concentrating until alcoholic smell is absent, adsorbing by using macroporous resin, eluting by using water and an ethanol solution, collecting eluent, concentrating to obtain an extract, dissolving the extract by adding alkali liquor, filtering, adding acid into filtrate to regulate the pH to be 2-4, filtering out a precipitate, and separating the precipitate by adopting high-performance countercurrent chromatography to obtain apigenin-7-O-beta-D-glucoside and vitexin. The preparation method is easy and convenient to implement and high in efficiency, and the product purity is high.

Description

Technical field: [0001] The invention relates to the field of pharmacy, in particular to a method for separating and purifying monomeric compounds from Rhizoma echinosum by applying macroporous resin adsorption method and high-speed countercurrent chromatography. Background technique: [0002] Coptidis macrophylla, also known as Coptis chinensis and Coptis chinensis, is the whole herb or rhizome of the Phytophthora spp., which is mainly distributed in the wetlands of the Yangtze River and southern Shaanxi forests or shrubs. It has the effects of clearing heat, detoxifying, dampness and stopping bleeding. It is used to treat wind-heat and cold, heat stroke, diarrhea, dysentery, white turbidity, leucorrhea, cough, hematemesis, blood in stool, hematuria, dental malnutrition, carbuncle swelling embolism. It mainly contains organic acids and flavonoids. It is clinically used to treat enteritis, hepatitis, pharyngitis and other diseases, and folkly used to treat gastric cancer, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08C07D407/04
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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