A kind of method for preparing Polygonum cuspidatum resveratrol and emodin

A technology of resveratrol and emodin, applied in chemical instruments and methods, preparation of organic compounds, pharmaceutical formulations, etc., can solve the problems of poor separation effect, no industrial value, limited separation accuracy, etc. The effect of normal coagulation, protection of hypoxic heart, and convenient operation

Active Publication Date: 2018-10-30
HUNAN XINLI BIOLOGICAL SCI & TECH +1
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

[0004] Existing methods for separating resveratrol and emodin from Polygonum cuspidatum, such as "Separation and Purification of Resveratrol with High Concentration Agarose Gel Microspheres" published in the "Abstracts of the 9th Session of the 28th Annual Academic Conference of the Chinese Chemical Society" in 2012 "The paper introduces the method for separating resveratrol from Polygonum cuspidatum with agarose gel microspheres. The defects of this method are: ① using acetic acid and ethanol aqueous solution as the mobile phase to separate resveratrol in the crude extract of Polygonum cuspidatum. On the basis of resveratrol, further separation of resveratrol and acetic acid is required
However, the concentration of acetic acid and ethanol in the recovery solution concentrated under reduced pressure has changed, so it must be recalibrated before each reuse, and the operation is cumbersome.
Another example is the article "Study on the Separation of Resveratrol in Polygonum cuspidatum by Gel Column Chromatography" published in Volume 21 of "Natural Product Research and Development" in 2009, which introduces the separation of resveratrol from Polygonum cuspidatum with Sephadex LH-20 gel. Method, the shortcoming of this method is: 1. directly separate with Polygonum cuspidatum thick extraction concentrate, because there is a large amount of impurity in the thick extraction concentrate of Polygonum cuspidatum, and gel chromatography only relies on the molecular diameter difference of isolate to realize separation, and separation precision is limited, Therefore, the separation effect is not good, and the purity of the isolated resveratrol only reaches 86.16%.
② After gel separation, the separation liquid has not been further refined and has no industrial value

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A method for preparing Polygonum cuspidatum resveratrol and emodin, its specific process steps are as follows:

[0029] (1) Preparation of MCI separation packing equilibrium column

[0030] Disperse the newly purchased MCI GEL CHP 20P with a particle size of 75-150 μm and the MCI GEL CHP20SS separation packing with a particle size of 63-150 μm in pure water, and then put it into a glass medium-pressure chromatography column with a diameter of 2 cm and a height of 50 cm , connect the constant flow pump, ultraviolet detector and partial collector, and assemble the MCI separation packed column system. Pumping volume concentration again is that 60% ethanol aqueous solution carries out equilibrium treatment, and this ethanol aqueous solution volume of pumping is 2 times of BV of MCI separation packed column volume, and the flow rate that pumps this ethanol aqueous solution is 2BV / h, and the ethanol aqueous solution that pumps into The pressure is 0.1MPa. Respectively colle...

Embodiment 2

[0042] A method for preparing Polygonum cuspidatum resveratrol and emodin, its specific process steps are as follows:

[0043] (1) Preparation of MCI separation packing equilibrium column

[0044] Disperse the newly purchased MCI GEL CHP 20P with a particle size of 75-150 μm and the MCI GEL CHP20SS separation filler with a particle size of 63-150 μm in pure water, and then put it into a glass medium-pressure chromatography column with a diameter of 5 cm and a height of 60 cm , connect the constant flow pump, ultraviolet detector and partial collector, and assemble the MCI separation packed column system. Pumping volume concentration again is that 70% ethanol aqueous solution carries out equilibrium treatment, and this ethanol aqueous solution volume of pumping is 3 times of BV of MCI separation packing column volume, and the flow rate that pumps this ethanol aqueous solution is 3BV / h, and the ethanol aqueous solution that pumps into The pressure is 0.15MPa. Respectively coll...

Embodiment 3

[0056] A method for preparing Polygonum cuspidatum resveratrol and emodin, its specific process steps are as follows:

[0057] (1) Preparation of MCI separation packing equilibrium column

[0058]Disperse the newly purchased MCI GEL CHP 20P with a particle size of 75-150 μm and the MCI GEL CHP20SS separation filler with a particle size of 63-150 μm in pure water, and then put it into a glass medium-pressure chromatography column with a diameter of 10 cm and a height of 80 cm , connect the constant flow pump, ultraviolet detector and partial collector, and assemble the MCI separation packed column system. Pumping volume concentration again is that 80% ethanol aqueous solution carries out equilibrium treatment, and this ethanol aqueous solution volume of pumping is 4 times of BV of MCI separation packed column volume, and the flow velocity that pumps this ethanol aqueous solution is 4BV / h, and the ethanol aqueous solution that pumps into The pressure is 0.2 MPa. Respectively c...

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Abstract

A method of preparing polygonum cuspidatum resveratrol and emodin belongs to the technical field of separation and preparation of the resveratrol and emodin. The method employs a polygonum cuspidatum resveratrol extract containing the emodin as a raw material, and includes the following steps: preparing a MCI separation filler equilibration column, preparing a polygonum cuspidatum resveratrol ethanol solution, preparing a resveratrol separation liquid, preparing concentrated liquids of the resveratrol and the emodin, preparing ethanol-removed concentrated liquids of the resveratrol and the emodin, and preparing freeze-dried powders of the resveratrol and the emodin, wherein the purity of the polygonum cuspidatum resveratrol is more than 99% and the purity of the emodin is more than 95%. Production devices in the method are all industrial devices. The method has mild production conditions and is suitable for large-scale production, and the product satisfies market demand. Through the membrane technology and a solvent recovery system, the method has low energy consumption and the material can be recycled, thereby significantly reducing production cost. The resveratrol and emodin products are widely used in the fields of medicines, health-caring foods, etc.

Description

1. Technical field [0001] The invention belongs to the technical field of separation and preparation of resveratrol and emodin, and in particular relates to a method for preparing polygonum cuspidatum resveratrol and emodin. 2. Background technology [0002] Resveratrol, referred to as stilbenol, is a non-flavonoid polyphenol compound containing stilbene structure, which is widely found in grapes, knotweed, peanuts and other plants. Biological and medical studies have shown that resveratrol has anti-oxidation, anti-aging, anti-tumor, anti-coagulation and coronary atherosclerosis, anti-inflammatory and anti-bacterial, prevention of high blood pressure and heart disease, improvement of blood circulation, lower blood sugar concentration, balance insulin Secretion, immune protection and other active effects, widely used in medicine, health food and cosmetics and other fields. Emodin is an anthraquinone compound, including macrocycline methyl ether, rhein, chrysophanol, emodin g...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A61K9/19A61K31/05A61K31/122A61P7/02A61P9/10A61P3/04A61P1/12A61P31/04A61P31/10A61P11/14A61P35/00A61P9/12C07C37/68C07C37/82C07C39/21C07C46/10C07C50/34
CPCA61K9/0019A61K9/19A61K31/05A61K31/122C07C37/685C07C37/82C07C46/10C07C39/21C07C50/34Y02P20/10
Inventor 杨洋袁德宽江文余红梅姚萍陶仁友黄国帅周小华
Owner HUNAN XINLI BIOLOGICAL SCI & TECH
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