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Method for modifying macroporous adsorption resin for separating and purifying resveratrol

A technology for separation and purification of resveratrol, applied in the separation/purification of hydroxyl compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of increasing difficulty, complicated pretreatment process, dead adsorption of silica gel, etc., and achieve easy industrialization Good production, separation and purification effects, and mild reaction conditions

Inactive Publication Date: 2013-08-28
CHONGQING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantages of this chromatographic column are: 1. the reutilization rate of alumina is low, which is not conducive to industrial production; silica gel can not be reused, causing a lot of waste in industrial production, and there is also dead adsorption in silica gel, which is not conducive to fully purifying Polygonum cuspidatum ②The separation effect of alumina or silica gel on resveratrol is not high, usually repeated column chromatography to achieve the desired purity, which makes the purification process complicated and the production cycle is long; ③Alumina and silica gel The pretreatment process is complex, which increases the difficulty of industrial production
The main disadvantage of this column chromatography packing is that it has poor adsorption to resveratrol, and most resins are only effective for certain types of traditional Chinese medicine ingredients, so that the adsorption rate of resveratrol is not high

Method used

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  • Method for modifying macroporous adsorption resin for separating and purifying resveratrol
  • Method for modifying macroporous adsorption resin for separating and purifying resveratrol
  • Method for modifying macroporous adsorption resin for separating and purifying resveratrol

Examples

Experimental program
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Effect test

Embodiment 1

[0023] The specific steps of a method for modifying a macroporous adsorption resin for separating and purifying resveratrol are as follows:

[0024] (1) Pretreatment of NKA-II resin

[0025] ①Alcohol wash and water wash

[0026]Using commercially available NKA-II resin as raw material, place the NKA-II resin in absolute ethanol at a ratio of 1:4 according to the mass (g) of NKA-II resin: the volume (mL) of absolute ethanol Soak for 24 hours to make the NKA-II resin soak and swell. Then use the conventional ethanol wet filling method to fill the soaked NKA-II resin into the chromatographic column, and then wash the chromatographic column filled with NKA-II resin with absolute ethanol at a speed of 2BV / h . Wash the NKA-II resin with alcohol to remove the residual organic solvent and residual monomer impurities in the polymerization reaction of the NKA-II resin during synthesis, and detect the effluent after alcohol washing (that is, in the detected effluent Add 4 times of di...

Embodiment 2

[0035] A method for modifying the macroporous adsorption resin used for separation and purification of resveratrol, same as embodiment 1, wherein:

[0036] In step (1)-①: the ratio of the mass of NKA-II resin (g): the volume of absolute ethanol (mL) is 1:3; soak in absolute ethanol for 22 hours; the speed of absolute ethanol is 1BV / h Rinse the chromatographic column filled with NKA-II resin; rinse the chromatographic column filled with NKA-II resin after washing with distilled water at a flow rate of 1BV / h.

[0037] In the 2nd (1)-2. step: the volume (mL) of the NKA-II resin after washing: the ratio of the volume (mL) of the hydrochloric acid solution that mass volume concentration is 4% is 1: 1; Described hydrochloric acid solution is 2mL / The chromatographic column packed with NKA-II resin after washing at the speed of min (1)-① step washing; NKA-II resin after pickling: mass volume concentration is that the volume ratio of 4% hydrochloric acid solution is 1: 1; soak the NK...

Embodiment 3

[0041] A method for modifying the macroporous adsorption resin used for separation and purification of resveratrol, same as embodiment 1, wherein:

[0042] In the 1st (1)-1. step: the quality (g) of NKA-II resin: the ratio of the volume (mL) of dehydrated alcohol is 1: 5; Soak 26h in dehydrated alcohol; Dehydrated alcohol is with the speed of 3BV / h Rinse the chromatographic column filled with NKA-II resin; wash the chromatographic column filled with NKA-II resin after washing with distilled water at a flow rate of 3BV / h.

[0043] In the 2nd (1)-2. step: the volume (mL) of the NKA-II resin after washing: the ratio of the volume (mL) of the hydrochloric acid solution that mass volume concentration is 6% is 1: 3; The chromatographic column that NKA-II resin is packed after the speed washing of the (1)-1. step washing at the speed of / min; : 3; the NKA-II resin after pickling was placed in the hydrochloric acid and soaked for 4h; the NKA-II resin after acid soaking was rinsed wit...

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Abstract

The invention discloses a method for modifying macroporous adsorption resin for separating and purifying resveratrol, and belongs to the technical field of preparation of adsorption resin. Commercial NKA-II resin is used as a raw material, and the product is obtained through a simple process of raw material pretreatment, chloromethylation reaction and aniline grafting. The method is simple, mild in reaction conditions, energy-saving, high in product yield and easy for realization of industrial production. The adsorption rate of the resveratrol adsorbed by the macroporous resin NKA-II-aniline modified by adopting the method reaches 99.59 percent. The method can be widely applied to modification of the macroporous resin, particularly NKA-II macroporous resin. The macroporous resin modified by adopting the method can be widely applied to separation and purification of active ingredients from natural medicinal plants, especially applied to separation and purification of the resveratrol from polygonum cuspidatum.

Description

technical field [0001] The invention belongs to the technical field of adsorption resin preparation, and in particular relates to a preparation method of an adsorption resin used for separating and purifying resveratrol from Polygonum cuspidatum. Background technique [0002] Polygonum cuspidatum is the rhizome of the perennial herb Polygonum cuspidatum, which is rich in resources. The active substance resveratrol is contained in the knotweed, and the content is relatively high. Resveratrol is a natural antioxidant that can reduce blood viscosity, inhibit platelet aggregation and vasodilation, keep blood flowing, prevent the occurrence and development of cancer, and have anti-atherosclerosis, coronary heart disease, ischemic Sexual heart disease, the prevention and treatment of hyperlipidemia, also has the effect of inhibiting tumor and estrogen, and can be used to treat diseases such as breast cancer. How to efficiently and easily separate and purify resveratrol from Poly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/285B01J20/30C07C39/21C07C29/76C08F12/08C08F8/24C08G73/02
Inventor 季金苟刘莉李祚丹徐溢穆小静
Owner CHONGQING UNIV
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