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Preparation method of rhapontin

A technology of rhubarb and rhubarb, applied in the preparation of rhubarb, using supercritical extraction technology combined with membrane separation technology to prepare rhubarb, which can solve the problems of low product purity, high energy consumption, and large solvent usage, etc. problem, to achieve the effect of simple operation of process steps and low energy consumption

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

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Problems solved by technology

The document "Study and Application of Active Components of Desmodium Glycyrrhizae and Rheum officinale" discloses that 90% ethanol is used for reflux extraction, after concentration, water is added to precipitate, and the precipitate is filtered out and dissolved in 95% ethanol. The solution is added to the activated carbon to absorb and remove impurities, and then purified by macroporous resin and recrystallization steps to obtain the product, this method uses multiple reflux extractions, which consumes a lot of energy, and the sample loss in the column operation is large
[0012] The document "HPLC Determination of Rhubarb Content in Hetao Rhubarb" uses 95% ethanol to extract and concentrate to obtain the total extract of rhubarb, and then repeatedly removes impurities from acid and alkali to obtain rhubarb. This method uses a large amount of solvent in the preparation process , and the product purity is not high
[0013] Patent "A Method for Extracting Rumex from Rumex" (Patent Publication No.: CN 101475613), the method used in this patent is to use Rumex as raw material, through crushing, heat reflux extraction, filtration, concentration, extraction , macroporous resin adsorption and eluting, concentrating, and drying to obtain rhubarb extract, and the method for preparing rhubarb consumes a lot of energy

Method used

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  • Preparation method of rhapontin

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Get 1kg of rhubarb rhubarb, pulverize, place in the extraction kettle, seal, set the temperature of the extraction kettle to be 45°C, the pressure to be 25MPa, the temperature of the separation kettle I to be 18°C, the pressure to be 15MPa, and the temperature of the separation kettle II to be 8°C. The pressure is 10MPa, turn on the extractor, separator and other devices to preheat the system, start the high-pressure pump, pass in 200ml of ethanol as a modifier, turn on the CO 2 Intake switch, start the compression pump, make the pressure reach the required range, keep the pressure for extraction for 1.5h, open the separation kettle I and separation kettle II, and carry out the separation operation, collect the extract, dissolve it with a sodium hydroxide solution of pH 9, and filter to remove the insoluble The solution is added to an ultrafiltration device with a pore size of 5nm for ultrafiltration. The permeate pressure is 0.5MPa. The permeate is concentrated through ...

Embodiment 2

[0026] Get 5kg of Tianshan rhubarb, pulverize, place in the extraction kettle, seal, set the temperature of the extraction kettle to be 35°C, the pressure to be 35MPa, the temperature of the separation kettle I to be 20°C, and the pressure to be 10MPa, the temperature of the separation kettle II to be 15°C, and the pressure to 6MPa, turn on the extractor, separator and other devices to preheat the system, start the high-pressure pump, feed 2.5L ethanol as a modifier, and turn on the CO 2 Intake switch, start the compression pump, make the pressure reach the required range, keep the pressure for extraction for 3 hours, open the separation kettle I and separation kettle II, carry out the separation operation, collect the extract, dissolve it with a potassium hydroxide solution of pH 11, and filter to remove the insoluble matter , the solution is added to an ultrafiltration device with a pore size of 15nm for ultrafiltration. The permeate pressure is 1MPa. The permeate is concentr...

Embodiment 3

[0028] Take 10kg of rhubarb in North China, pulverize it, put it in the extraction kettle, seal it, set the temperature of the extraction kettle to 38°C, the pressure to 28MPa, the temperature of the separation kettle I to 20°C, the pressure to 13MPa, the temperature of the separation kettle II to 12°C, and the pressure to 8MPa, turn on the extractor, separator and other devices to preheat the system, start the high-pressure pump, feed 3L ethanol as a modifier, and turn on the CO 2 Intake switch, start the compression pump, make the pressure reach the required range, keep the pressure for extraction for 2.5h, open the separation kettle I and separation kettle II, and carry out the separation operation, collect the extract, dissolve it with a sodium hydroxide solution of pH 10, and filter to remove the insoluble The solution is added to an ultrafiltration device with a pore size of 10nm for ultrafiltration. The permeate pressure is 0.8MPa. The permeate is concentrated through a ...

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Abstract

The invention relates to a preparation method of rhapontin. The preparation method comprises: crushing dried Polygonaceae Rheum herbs into coarse powder, placing the coarse powder in an extraction kettle for supercritical CO2 extraction, collecting the extract in a separation kettle, adding a base liquid for dissolving, filtering out insoluble substances, filtering the filtrate through an ultrafiltration membrane, collecting the permeate liquid, then concentrating the collected liquid by use of a nanofiltration membrane, adjusting the pH value of the concentrate for crystallization, filtering out the crystal, and recrystallizing by virtue of ethanol and water to obtain a product. The preparation method of rhapontin provided by the invention has the advantages of simplicity in technological operation, low energy consumption and easiness for realization of industrial production; and the obtained product is high in purity.

Description

Technical field: [0001] The invention belongs to the field of biotechnology, and in particular relates to a method for preparing rhubarb, in particular to a method for preparing rhubarb by using supercritical extraction technology combined with membrane separation technology. Background technique: [0002] Earth rhizoma glucoside: [0003] Properties: white needle-like crystal, blue fluorescence under ultraviolet light (254mn), FeCl 3 The reaction is blue-black; [0004] English name: (rhaponticin, rhaponitin or poniticin); [0005] Chemical name: 3-hydroxy-5-[(1E)-2-(3-hydroxy-4-methoxyphenyl)vinyl]phenyl-β-D-glucoside; [0006] Molecular formula: C 21 h 24 o 9 [0007] Molecular weight: 420; [0008] Structural formula: [0009] [0010] Rhubarb is a derivative of stilbene. Mainly found in Polygonaceae Rhubarb plants. The Chinese Pharmacopoeia 2005 edition one part stipulates that no rhubarb can be detected under the item of rhubarb, and it is generally belie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/203C07H1/08
CPCY02P20/54
Inventor 刘东锋吴艳波杨成东
Owner NANJING ZELANG MEDICAL TECH
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