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Method for rapid separation and preparation of stilbene glycosides from Radix Polygoni Multiflori

A technology for stilbene glycosides and crude stilbene glycosides is applied in the field of ultrasonic extraction and medium pressure preparative chromatography for rapid separation and purification of stilbene glycosides, and can solve the problems of stilbene glycosides destruction, increased preparation cost, large sample loss and the like , to achieve the effect of low production cost, avoiding target loss and easy operation

Inactive Publication Date: 2015-09-23
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 rapid separation and preparation of stilbene glycosides from Radix Polygoni Multiflori
  • Method for rapid separation and preparation of stilbene glycosides from Radix Polygoni Multiflori

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Effect test

Embodiment 1

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

[0024] (1) Preparation of raw material extract

[0025] The decoction pieces of Radix Polygoni Multiflori are used as raw materials, and 60% dilute ethanol is used as the extraction solvent. First put the raw materials into a pulverizer for pulverization, and pass through an 80-mesh iron sieve to collect the sieved raw material powder, and then put the raw materials that have not been sifted into the pulverizer for pulverization. Then, according to the ratio of the mass (g) of the raw material powder: the volume (mL) of dilute ethanol as the ratio of 1:10, the raw material powder and dilute ethanol are placed in the ultrasonic extractor, first stirred and mixed evenly, and then the ultrasonic power is 300W 1. Under the conditions of ultrasonic working frequency of 40KHZ and temperature of 60°C, after the first ultrasonic extract...

Embodiment 2

[0033] A method for rapidly separating stilbene glycosides in Radix Polygoni Multiflori by medium-pressure preparative chromatography, the same as in Example 1, wherein:

[0034] In step (1): After 500.0 g of Radix Polygoni Multiflori medicinal material is pulverized, pass through a 100-mesh sieve, and the medicinal material powder after sieving and 50% dilute ethanol solution are according to the mass (g) of raw material powder: the ratio of the volume (mL) of dilute ethanol 1:8, under the conditions of ultrasonic power of 500W, ultrasonic working frequency of 50KHZ, and extraction temperature of 70°C, extraction was performed for 1.0h, and this was repeated twice to prepare the raw material extract I.

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

Embodiment 3

[0039] A method for rapidly separating stilbene glycosides in Radix Polygoni Multiflori by medium-pressure preparative chromatography, the same as in Example 1, wherein:

[0040] In step (1): after pulverizing 500.0 g of Radix Polygoni Multiflori medicinal material, pass through a 60-mesh sieve, and the medicinal material powder after sieving and 40% dilute ethanol solution are according to the mass (g) of raw material powder: the ratio of the volume (mL) of dilute ethanol 1:15, added to the ultrasonic extraction device, under the conditions of ultrasonic power of 350W, ultrasonic operating frequency of 40KHZ, and extraction temperature of 65°C, after ultrasonic extraction for 1.5h, the operation was repeated twice to prepare the raw material extract I .

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

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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, and in particular relates to a method for ultrasonically extracting and medium-pressure preparation chromatographic rapid separation and purification of stilbene glycosides from Polygonum multiflorum medicinal material. Background technique [0002] Stilbene glycosides, also known as stilbene polyphenols, belong to polyhydroxy stilbene compounds. Stilbene glycosides are unique biologically active ingredients in Polygonum multiflorum, and are the specific index components of Polygonum multiflorum. They are easily soluble in water, methanol, and ethanol. Pharmacological studies have shown that stilbene glycosides have the functions of anti-oxidation, scavenging free radicals, anti-aging, lowering cholesterol, protecting the liver and protecting nerves, and can be developed to develop new drugs for the treatment of senile dementia, lowering blood fat and anti-...

Claims

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Application Information

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