Method for extraction and separation of verbascoside from rehmannia glutinosa

A technology of verbascoside and Rehmannia glutinosa, applied in chemical instruments and methods, sugar derivatives, sugar derivatives and other directions, can solve the problems of large solvent consumption and long time consumption, and achieve the effects of saving resources, high speed and controllable operation.

Inactive Publication Date: 2016-11-02
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] After reviewing the literature, it is found that there are already many methods for the separation and purification of verbascoside compounds, such as extracting and separating verbascoside from the flowers of Aurantia nudica, Cistanche, Osmanthus fragrans, and Paulownia tomentosa. These separation and purification processes mainly use repeated column chromatography to obtain high-purity The acteoside samples of these plants have defects such as long time-consuming and large solvent consumption in the repeated chromatography process; in addition, there are many literature reports using high-performance liquid chromatography to analyze the contents of acteoside in these plants
At present, there is no literature report on an efficient method for the preparative separation and purification of verbascoside from Rehmannia glutinosa

Method used

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  • Method for extraction and separation of verbascoside from rehmannia glutinosa
  • Method for extraction and separation of verbascoside from rehmannia glutinosa
  • Method for extraction and separation of verbascoside from rehmannia glutinosa

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Embodiment 1

[0033] Extraction: Weigh 300g of rehmannia medicinal material, put it in a 1000ml round bottom flask, add 500ml of ethanol solution with a volume fraction of 75%, heat and reflux for extraction, the number of extractions is 2 times, and each time is 1.5h. Combine the extracts, cool, filter, move the filtrate to a 1000ml flask, spin dry with a rotary evaporator to obtain an extract. Enrichment of verbascoside with macroporous resin: Take a certain amount of pretreated D101 macroporous resin, pack it into a column, take the extract and dilute it with water and load it as a sample, and control the flow rate at 4BV / h until the adsorption is complete. Then carry out gradient elution, first elution with water to remove sugars, and then sequentially elution with 5%, 10%, 20% volume concentration of ethanol aqueous solution, each gradient elution, when the effluent is colorless, you can replace the next one Gradient, collect the eluate eluted with 5% ethanol aqueous solution, and conc...

Embodiment 2

[0035]Extraction: Weigh 300g of rehmannia medicinal material, put it in a 1000ml round bottom flask, add 500ml of 75% ethanol solution, heat and reflux for extraction twice, each time is 1.5h. Combine the extracts, cool, filter, move the filtrate to a 1000ml flask, spin dry with a rotary evaporator to obtain an extract. Macroporous resin enrichment of verbascoside: take a certain amount of pretreated D101 resin (equivalent to 10g dry resin), pack it into a column, dilute the total extract of Rehmannia glutinosa with water as the loading solution, and control the flow rate of the resin column to 4BV / h until the adsorption is complete. Then carry out gradient elution, first elution with water to remove sugar components, and then sequentially elution with 10%, 20% volume concentration of ethanol aqueous solution, during each gradient elution, when the effluent is colorless, the next gradient can be replaced. The eluate eluted with 10% ethanol aqueous solution was collected and s...

Embodiment 3

[0037] Extraction: Weigh 300g of rehmannia medicinal material, put it in a 1000ml round bottom flask, add 500ml of 75% ethanol solution, heat and reflux for extraction twice, each time is 1.5h. Combine the extracts, cool, filter, move the filtrate to a 1000ml flask, spin dry with a rotary evaporator to obtain an extract. Enrichment of verbascoside with macroporous resin: Take a certain amount of pretreated D101 resin (equivalent to 10g dry resin), pack it into a column, dilute the total extract of Rehmannia glutinosa and load the sample, control the flow rate of the resin column to 4BV / h until the adsorption completely. Then carry out gradient elution, first elution with water to remove sugar components, and then sequentially elution with 5%, 10%, 20% volume concentration of ethanol aqueous solution, during each gradient elution, the effluent can be replaced when it is colorless A gradient, collect the eluate eluting with 5% and 10% ethanol aqueous solution, combine, see the ...

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Abstract

The invention discloses a method for extraction and separation of verbascoside from rehmannia glutinosa. The method consists of: using a 75% ethanol aqueous solution to conduct heating reflux extraction on dried raw rehmannia root to obtain rehmannia root total extract, carrying out macroporous adsorption resin separation and gradient elution on the rehmannia root total extract, collecting 5-10% ethanol eluent to prepare a verbascoside crude product, and then performing separation and purification by high-speed counter-current chromatography so as to obtain a verbascoside pure product. The method provided by the invention utilizes macroporous resin to acquire a 5-10% ethanol eluent enriched material, makes full use of crude drug resources, employs high-speed counter-current chromatography for separation and purification to obtain the verbascoside standard product, realizes automation and operability of a monomer purification process, can obtain a monomer finished product with purity up to 98% or more, and has the characteristics of convenience and simplicity, high product purity, resource saving, fast speed, low toxicity, and controllable operation, etc.

Description

(1) Technical field [0001] The invention relates to a method for extracting and separating pure verbascoside from Chinese medicine rehmannia glutinosa. (2) Background technology [0002] Rehmannia glutinosa (scientific name: Rehmannia glutinosa) is the fresh or dried root tuber of Rehmannia glutinosa, a plant of the family Scrophulariaceae. Widely distributed in Henan, Hubei, Shanxi, Sichuan, Zhejiang, Inner Mongolia, Hunan, Shandong, Liaoning and other provinces and cities in China. Fresh Rehmannia glutinosa is cold in nature, sweet and bitter in taste, and has the effects of clearing heat and promoting body fluid, cooling blood, and stopping bleeding; raw rehmannia glutinosa is cold in nature, sweet in taste, has the effects of clearing heat and cooling blood, nourishing yin, and promoting body fluid; rehmannia glutinosa is slightly warm in nature, sweet in taste, and has the effect of nourishing yin and nourishing blood. , The effect of benefiting the essence and filling...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/18C07H1/08
Inventor 童胜强步知思李行诺楚楚
Owner ZHEJIANG UNIV OF TECH
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