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Method for preparing stibene glucoside from polygonum multiflorum by rapid separation

A technology for stilbene glycosides and crude stilbene glycosides, which is applied in the field of ultrasonic extraction and medium-pressure preparative chromatography for rapid separation and purification of stilbene glycosides, which can solve the problems of stilbene glycoside damage, increased preparation costs, and large solvent consumption, etc. problems, to achieve low production costs, avoid target loss, and shorten extraction time

Inactive Publication Date: 2014-02-12
CHONGQING UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantages of this method are: ① high temperature reflux is used to extract stilbene glycosides, which are easily oxidized and glycosidic bonds are broken under high temperature conditions, and this extraction method causes damage to stilbene glycosides; ② normal pressure column chromatography is used Multiple separations, the process is cumbersome, time-consuming, solvent consumption is large, and the preparation cost is increased; ③The component stays in the column at atmospheric pressure for too long, resulting in dead adsorption, large sample loss, and low recovery rate

Method used

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  • Method for preparing stibene glucoside from polygonum multiflorum by rapid separation
  • Method for preparing stibene glucoside from polygonum multiflorum by rapid separation

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Experimental program
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Effect test

Embodiment 1

[0023] The specific steps of a method for rapidly separating stilbene glycosides from Polygonum multiflorum medicinal materials are as follows:

[0024] (1) Preparation of raw material extract

[0025] The raw material of the raw materials of Polygonum multiflorum is decoction pieces, and 60% dilute ethanol is used as the extraction solvent. First put the raw materials into the pulverizer for pulverization, and sieve them through an 80-mesh iron sieve, collect the sieved raw material powder, and put the unscreened raw materials into the pulverizer for pulverization. Then according to the ratio of the mass (g) of the raw material powder: the volume (mL) of the dilute ethanol is 1:10, the raw material powder and the dilute ethanol are placed in the ultrasonic extractor, first stirred and mixed evenly, and then the ultrasonic power is 300W , Under the conditions of ultrasonic working frequency of 40KHZ and temperature of 60℃, after the first ultrasonic extraction for 0.5h, the e...

Embodiment 2

[0033] A method for rapidly separating stilbene glycosides in Polygonum multiflorum using medium pressure preparative chromatography, with embodiment 1, wherein:

[0034] In step (1): After crushing 500.0g of Polygonum multiflorum medicinal material, pass it through a 100-mesh sieve. The sieved medicinal material powder and 50% dilute ethanol solution are in the ratio of the mass (g) of the raw material powder: the volume (mL) of the dilute ethanol 1:8, under the condition of ultrasonic power of 500W, ultrasonic operating frequency of 50KHZ, and extraction temperature of 70°C, extraction was performed for 1.0h, and this was repeated twice to prepare raw material extract I.

[0035] In the (2) step: the ratio of the mass (g) of the raw material extract: the volume (mL) of the petroleum ether is 1:10, in the water bath environment of 95 ° C, reflux extraction 0.5h, repeat the operation 2 times , the raw material extract II of degreasing treatment was obtained.

[0036] In the (...

Embodiment 3

[0039] A method for rapidly separating stilbene glycosides in Polygonum multiflorum using medium pressure preparative chromatography, with embodiment 1, wherein:

[0040] In step (1): After crushing 500.0g of Polygonum multiflorum medicinal material, pass it through a 60-mesh sieve. The sieved medicinal material powder and 40% dilute ethanol solution are in the ratio of the mass (g) of the raw material powder: the volume (mL) of the dilute ethanol The ratio of 1:15 was added to the ultrasonic extraction device, and the ultrasonic power was 350W, the ultrasonic operating frequency was 40KHZ, and the extraction temperature was 65°C. After ultrasonic extraction for 1.5h, the operation was repeated 2 times to prepare the raw material extract I. .

[0041] In the (2) step: the ratio of the mass (g) of the raw material extract: the volume (mL) of the petroleum ether is 1:5, in a water bath environment of 60 ° C, reflux extraction 1.5h, repeat the operation 2 times , the raw materia...

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Abstract

The invention relates to a method for preparing stibene glucoside from polygonum multiflorum by rapid separation and belongs to the technical field of extraction and separation of stibene glucoside. According to the invention, the stibene glucoside product is prepared by using raw polygonum multiflorum as the raw material through the steps of preparing extract of the raw material, degreasing the extract of the raw material and preparing a crude product and a fine product of stibene glucoside. The method has the characteristics of high extraction efficiency, simple separation preparation process, rapid and time-saving separation process, high purity and good reproducibility of the prepared product, sufficient utilization of the raw material, low production cost and the like. The method can be widely applied to preparation of the stibene glucoside product from polygonum multiflorum by separation and can effectively meet the requirement on preparation of a high-purity sample in the conventional pharmacodynamic experimental research.

Description

technical field [0001] The invention belongs to the technical field of extraction and separation of stilbene glycosides, in particular to a method for ultrasonic extraction and medium pressure preparative chromatography for rapid separation and purification of stilbene glycosides from the medicinal materials of Polygonum multiflorum. Background technique [0002] Stilbene glycosides, also known as stilbene polyphenols, belong to polyhydroxy stilbene compounds. Stilbene glycosides are the unique bioactive components of Polygonum multiflorum medicinal materials, and are the exclusive index components of Polygonum multiflorum medicinal materials. They are easily soluble in water, methanol and ethanol. Pharmacological studies have shown that stilbene glycosides have anti-oxidative scavenging free radicals, anti-aging, lowering cholesterol, protecting liver and neuroprotection, and can develop new drugs for the treatment of senile dementia, blood lipid lowering and anti-atheroscle...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/18C07H1/08
Inventor 徐溢张庆曹坤邹胜
Owner CHONGQING UNIV