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Flavone magnetic molecularly imprinted polymer, preparation of flavone magnetic molecularly imprinted polymer, and application of flavone magnetic molecularly imprinted polymer to bamboo-leaf flavone separation

A technology of magnetic molecular imprinting and bamboo leaf flavonoids, which is applied in the directions of alkali metal compounds, separation by moving adsorbents, and other chemical processes, etc., can solve problems such as difficulty in meeting the demand for high-content bamboo leaf flavonoids products.

Inactive Publication Date: 2012-09-12
INT CENT FOR BAMBOO & RATTAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Bamboo leaf flavone products currently on the market are mainly crude products, and the total content of the above four flavonoids is generally within 10%, which is difficult to meet the market demand for high-content bamboo leaf flavonoid products

Method used

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  • Flavone magnetic molecularly imprinted polymer, preparation of flavone magnetic molecularly imprinted polymer, and application of flavone magnetic molecularly imprinted polymer to bamboo-leaf flavone separation
  • Flavone magnetic molecularly imprinted polymer, preparation of flavone magnetic molecularly imprinted polymer, and application of flavone magnetic molecularly imprinted polymer to bamboo-leaf flavone separation
  • Flavone magnetic molecularly imprinted polymer, preparation of flavone magnetic molecularly imprinted polymer, and application of flavone magnetic molecularly imprinted polymer to bamboo-leaf flavone separation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1. Preparation of Flavone Magnetic Molecularly Imprinted Polymer Microspheres (the molar ratio of template molecule to functional monomer is 1:5)

[0031] ⑴ Accurately pipette 36mlL (1molL -1 ) FeCl 3 and 40mlL (1molL -1 ) mixed solution of HCl, was added to a 500mL three-necked flask, pumped with a vacuum pump, and then passed nitrogen for 30min to remove the air in the three-necked flask, and then weighed 0.02mol, that is, 5.5604g FeSO 4 ·7H 2 O was quickly added to the three-necked flask (molar ratio Fe 3+ : Fe 2+ =1.8∶1), when FeSO 4 ·7H 2 After O is completely dissolved, add 25mL (10%) of PEG4000 solution, drop 1.5molL -1 NaOH solution, adjust the pH to 10. Pass nitrogen to replace and remove oxygen, heat up to 70°C, and rotate at 800r min -1 , after rapid stirring for 10 minutes, reduce the stirring speed to 500r·min -1 At the same time, the temperature was raised to 80°C for constant temperature reaction for 1h. After the reaction, the solid-liq...

Embodiment 2

[0035] Example 2. Preparation of Flavone Magnetic Molecularly Imprinted Polymer Microspheres (the molar ratio of template molecule to functional monomer is 1:8)

[0036] (1) surface-modified Fe is prepared by the method of embodiment 1 3 o 4 particle.

[0037] (2) Prepare 120mL of polyethylene glycol aqueous solution with a concentration of 3%~3.5%; add 3.5g of nano-Fe modified by oleic acid 3 o 4 Particles; 8mmol functional monomer 4-vinylpyridine (4-vp) and 0.1431g (1mmol) template molecule luteolin were dissolved in polyethylene glycol solution; 7.5mL cross-linking agent ethylene dimethacrylate Alcohol ester (EGDMA), 0.25g initiator azobisisobutyronitrile (AIBN) were dissolved in 7.5mL xylene; the above-mentioned mixed solution was transferred to a 500mL three-necked flask, and ultrasonically degassed for 10min; ℃, 300rpm and constant temperature stirring for 15h.

[0038] (3) After the reaction, under the action of an external magnetic field, separate the polymer micr...

Embodiment 3

[0039] Example 3. Application of flavone magnetic molecularly imprinted polymers in the separation of flavonoids from bamboo leaves

[0040] (1) Weigh 100g of dried moso bamboo leaf samples, add 95% ethanol according to the solid-liquid ratio of 1:10, and prepare bamboo leaf flavonoid extract. Six standard substances of luteolin, orientin, isoorientin, vitexin, isovitexin and quercetin were added to the extract;

[0041] (2) Weigh 250 mg of the prepared magnetic molecularly imprinted polymers (MMIPs) and place them in a 100 mL Erlenmeyer flask.

[0042] (3) Pipette 50 mL of the bamboo leaf extract prepared in step (1), add it into the Erlenmeyer flask filled with MMIPs, and shake and extract at room temperature at 150 rpm for 210 min.

[0043] (4) Separation of solid and liquid under the action of an external magnetic field, add 10mL of 10% ethanol solution to rinse for 3 times, after magnetic separation, add 10mL of methanol: acetic acid (formic acid) = 9:1 (8:2) solution, s...

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Abstract

Flavone magnetic molecularly imprinted polymer, preparation of the flavone magnetic molecularly imprinted polymer, and application of the flavone magnetic molecularly imprinted polymer to bamboo-leafflavone separation belong to the technical field of drug separation. Preparation of flavone magnetic molecularly imprinted polymer microspheres include subjecting nano Fe3O4 subjected to surface modification by oleic oil, template molecule luteolin, functional monomer 4-ethylpyridine and cross linking agent ethylene glycol dimethacrylate to suspension polymerization according to a template molecule, functional monomer and crosslinking agent ratio of 1:5-8:80. The flavone magnetic molecularly imprinted polymer microspheres are applicable to selective enrichment and purification of bamboo-leaf flavones in bamboo-leaf extract, and the preparation is simple, quick, high in recovery rate and the like and is widely applicable to the field of separation of natural flavone compounds.

Description

technical field [0001] The invention belongs to the technical field of medicine separation, and in particular relates to flavonoid magnetic molecularly imprinted polymer microspheres for highly selective separation, purification and enrichment of flavonoids in bamboo leaf extracts, a preparation method and application. Background technique [0002] The classic preparation method of bioactive ingredients mainly uses organic solvent extraction, and then further purification by separation techniques such as column chromatography and recrystallization. There are many and complicated extraction steps, high production costs, large consumption of organic solvents, and easy to cause solvent residues and environmental pollution issues. For complex matrices such as fermentation broth and plant extracts, separation by silica gel and adsorption resin column chromatography will cause column contamination, and centrifugation and filtration cannot separate the adsorbed target components fr...

Claims

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Application Information

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IPC IPC(8): C08F222/14C08F226/06C08F2/44C08J9/26C08K9/04C08K3/22B01J20/26B01J20/28B01J20/30B01D15/02
Inventor 汤锋王光勇岳永德王进姚曦郭雪峰孙嘏
Owner INT CENT FOR BAMBOO & RATTAN
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