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Method for separating stilbene effective components out from stem and bark of acanthopanax leucorrhizus

A technology for the separation of active ingredients, applied in the field of extraction of active ingredients from Chinese herbal medicines, can solve the problems of limited system research and development, difficulty in separation and structure identification, and low content of stilbene compounds, achieving good reproducibility and reducing labor intensity And the loss of active ingredients, the effect of a large amount of extraction

Inactive Publication Date: 2018-07-13
EASTERN GANSU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the low content of most stilbene compounds in nature, it is difficult to separate and identify their structures, which limits their systematic research and development.
[0003] At present, the separation methods for stilbene components are mainly traditional solvent-assisted various chromatography methods (such as silica gel column chromatography, polyamide column chromatography, preparative thin-layer chromatography, ODS, Sephadex LH-20 column chromatography and HPLC, etc.), but All have the disadvantages of complex process, long cycle, large solvent consumption, low extraction rate and low purity to varying degrees.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1 A kind of method for isolating the active ingredient of stilbene class from the stem bark of Radix Acanthopanax, comprising the following steps:

[0026] (1) After drying, pulverizing and passing 40 mesh sieves of 300 g of fresh vine root bark, vine root bark powder is obtained, and the volume concentration of 10 mL / g is added into the vine root bark powder according to the liquid-solid ratio 75% ethanol, placed in a stirrer magnet, placed in a microwave extractor, at a stirring speed of 600 rpm, an extraction temperature of 60 °C, a microwave power of 700 W, an extraction time of 15 min, and extraction times of 2 Under the conditions of microwave extraction, the extract was obtained; the extract was concentrated under reduced pressure at a pressure of 0.05 MPa, a temperature of 40 °C, and a rotation speed of 100 rpm to obtain a crude extract.

[0027] (2) Extract the crude extract three times with petroleum ether and ethyl acetate in order of 3 times the v...

Embodiment 2

[0037] Embodiment 2 A kind of method for isolating the active ingredient of stilbene class from the stem bark of Radix Acanthopanax, comprising the following steps:

[0038] (1) After drying 500 g of fresh vine root bark, pulverizing and passing through a 50-mesh sieve, the vine root bark powder is obtained, and the volume concentration of 15 mL / g is added into the vine root bark powder according to the liquid-solid ratio 80% ethanol was put into a stirrer magnet, placed in a microwave extractor, and the stirring speed was 650 rpm, the extraction temperature was 60 °C, the microwave power was 650 W, the extraction time was 20 min, and the number of extractions was 3 times. Microwave extraction was carried out under certain conditions to obtain an extract; the extract was concentrated under reduced pressure at a pressure of 0.06 MPa, a temperature of 50 °C, and a rotation speed of 150 rpm to obtain a crude extract.

[0039] (2) Extract the crude extract three times with petrole...

Embodiment 3

[0048] Embodiment 3 A kind of method for isolating the active ingredient of stilbene class from the stem bark of Radix Acanthopanax, comprising the following steps:

[0049] (1) After drying 400 g of fresh vine root bark, crushing and passing through a 60-mesh sieve, vine root bark powder is obtained, and the volume concentration of 20 mL / g is added into the vine root bark powder according to the liquid-solid ratio 95% ethanol was put into a stirrer magnet, placed in a microwave extractor, and the stirring speed was 700 rpm, the extraction temperature was 65 °C, the microwave power was 750 W, the extraction time was 20 min, and the number of extractions was 3 times. Under the conditions of microwave extraction, the extract was obtained; the extract was concentrated under reduced pressure at a pressure of 0.055 MPa, a temperature of 45 °C, and a rotation speed of 125 rpm to obtain a crude extract.

[0050] ⑵The crude extract was sequentially extracted 4 times with petroleum eth...

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PUM

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Abstract

The invention relates to a method for separating stilbene effective components out from stem and bark of acanthopanax leucorrhizus. The method comprises the following steps: (1) drying the stem and bark of the fresh acanthopanax leucorrhizus in the air, crushing, sieving, and then carrying out microwave extraction and vacuum concentration to obtain a crude extract; (2) sequentially extracting thecrude extract with petroleum ether and ethyl acetate until extract liquor becomes colorless, merging the ethyl acetate extract liquor, and drying by distillation under the reduced pressure to obtain asample to be separated; (3) ultrasonically dissolving the sample to be separated with a mixed solvent to obtain a sample solution; (4) determining a preparative high-speed countercurrent chromatography (HSCCC) two-phase solvent system; (5) after a stationary phase and a mobile phase are separately degassed ultrasonically, sequentially pumping the products into multiple layers of spiral tubes of apreparative countercurrent chromatograph, and then injecting the sample solution for performing purification and separation; (6) sequentially collecting seven chromatographic peak components according to a chromatogram, and enabling the seven components to be separately subjected to vacuum concentration and vacuum drying so as to obtain seven stilbene compounds. The method provided by the invention is simple and easy to implement, high in extraction amount and good in reproducibility; the purities of the seven obtained stilbene compounds are higher than 98.0%.

Description

technical field [0001] The invention relates to the technical field of extraction of effective components of traditional Chinese medicinal materials, in particular to a method for isolating effective components of stilbenes from stem bark of Acanthopanax vine. Background technique [0002] Fuji five plus ( Acanthopanax leucorrhizus ) belongs to the small perennial deciduous shrub of the genus Acanthopanax. It is a unique folk medicinal plant in my country, mainly distributed in Shaanxi, Gansu, Yunnan, Guizhou, and the middle and lower reaches of the Yangtze River. Its medicinal parts are mainly root bark and stem bark, which have the functions of dispelling rheumatism, dredging meridian, strengthening scorpion, etc. Wet swelling embolism. The main medicinal components of the stem bark of vine root are stilbenes, flavonoids, phenylpropanoids, terpenoids, lignans, coumarins, polysaccharides and other components. The study found that part of the stilbene components isolated ...

Claims

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Application Information

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IPC IPC(8): C07D313/14C07C41/34C07C41/36C07C43/23C07C43/215C07C37/70C07C37/82C07C39/21C07D307/83
CPCC07B2200/09C07C37/70C07C37/82C07C41/34C07C41/36C07D307/83C07D313/14C07C43/23C07C43/215C07C39/21
Inventor 胡浩斌梁海鹏李海明袁如楠韩明虎张腊腊武芸
Owner EASTERN GANSU UNIVERSITY
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