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Method for extracting harpagoside

A technology for extracting harpagoside and solvent, which is applied in the field of natural medicinal chemistry to achieve the effects of increased yield, simple operation, and easy scale-up

Inactive Publication Date: 2012-03-14
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] At present, there are few existing methods for extracting harpagoside, most of which are crude extracts

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take fresh Scrophulariaceae, crush it, take 1kg, put it into a flask, add 5L of 60% methanol, reflux extraction for 2 hours, release the liquid, add an equal volume of methanol for reflux extraction twice, combine extraction and filtration, reduce pressure in a rotary evaporator without alcohol After adding an appropriate amount of water to disperse, add 500ml polyamide resin column for adsorption, after the adsorption is completed, use 5L water → 2L 30% methanol solution → 3.5L 50% methanol solution for elution, collect 50% methanol eluate and concentrate under reduced pressure to a density of 1.1 to obtain Put 50ml of the liquid into a separatory funnel, add 100ml of ethyl acetate to fully shake, extract 6 times, combine the ethyl acetate layer and recover it under reduced pressure until 100ml is released, pour it into a conical flask, add 20ml of petroleum ether, stir evenly and place it to crystallize. Filter out the crystals, dissolve them under reflux with methanol...

Embodiment 2

[0025] Take fresh Scrophulariaceae, crush it, take 1kg, put it into a flask, add 5L of 60% ethanol, reflux extraction for 2 hours, release the liquid, add an equal volume of ethanol for reflux extraction twice, combine extraction and filtration, reduce pressure in a rotary evaporator without alcohol After adding an appropriate amount of water to disperse, add 500ml polyamide resin column for adsorption. After the adsorption is over, use 5L water → 2L 30% ethanol solution → 3.5L 50% ethanol solution for elution, collect the 50% ethanol eluate and concentrate it under reduced pressure to a density of 1.1 to obtain Put 50ml of the liquid into a separatory funnel, add 100ml of ethyl acetate to fully shake, extract 6 times, combine the ethyl acetate layer and recover it under reduced pressure until 100ml is released, pour it into a conical flask, add 20ml of petroleum ether, stir evenly and place it to crystallize. Filter out the crystals, dissolve them with methanol under reflux, a...

Embodiment 3

[0027] Take fresh Scrophulariaceae, crush it, take 1kg, put it into a flask, add 5L of 70% acetone, reflux extraction for 2 hours, release the liquid, add an equal volume of acetone for reflux extraction twice, combine extraction and filtration, and recover under reduced pressure in a rotary evaporator. After adding an appropriate amount of water to disperse, add 500ml polyamide resin column for adsorption. After the adsorption is completed, use 5L water-→2L 30% methanol solution→3.5L 50% methanol solution for elution, collect 50% methanol eluate and concentrate under reduced pressure to a density of 1.1 to obtain Put 50ml of the liquid into a separatory funnel, add 100ml of ethyl acetate to fully shake, extract 6 times, combine the ethyl acetate layer and recover it under reduced pressure until 100ml is released, pour it into a conical flask, add 20ml of petroleum ether, stir evenly and place it to crystallize. Filter out the crystals, dissolve them under reflux with methanol,...

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PUM

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Abstract

The invention discloses a method for extracting harpagoside. The method includes the following steps: fresh figwort roots as a raw material are ground and then added with methanol, ethanol or acetone aqueous solution for reflux extraction, extract is added into a polyamide column for separation after the reagent is recovered, 5 to 10 BV water, 20 to 30 percent of 4 to 6 BV ethanol (methanol) solution and 50 to 70 percent of 5 to 7 BV ethanol (methanol) solution are sequentially used for elution, eluent is concentrated and then extracted with ethyl acetate for 4 to 6 times, extract is concentrated and added with petroleum ether for crystallization, methanol-chloroform mixture is then added for recrystallization, and after low-temperature drying, the harpagoside is obtained. The repeatability of the process is high, and the method is suitable for the production of high-content harpagoside.

Description

Technical field: [0001] The invention belongs to the field of natural medicinal chemistry, and in particular relates to a method for extracting harpagoside. Background technique: [0002] Harpagosides, iridoid glycosides. [0003] Molecular formula: C 19 h 18 o 8 ; [0004] Physical and chemical properties: light yellow crystal (methanol), mp.189~190℃. [0005] Harpagoside has anti-inflammatory, antihypertensive, and anti-hepatitis B virus effects. [0006] Scrophulariaceae is the dry root of the plant Scrophulariaceae Scrophulariaceae. It tastes sweet, bitter, salty, and slightly cold in nature. It returns to the lung and stomach meridian. It has the effects of cooling blood and nourishing yin, purging fire and detoxifying. , red eyes, sore throat, scrofula, diphtheria, carbuncle sores embolism. Its chemical composition mainly includes iridoid glycosides, phenylpropanoids, triterpenoid saponins, organic aromatic acids, flavonoids, fatty acids and volatile oils. [...

Claims

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Application Information

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IPC IPC(8): C07H17/04C07H1/08
Inventor 李法庆杨成东刘东锋
Owner 苏州宝泽堂医药科技有限公司
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