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Preparation method and application of benzophenanthridine alkaloid molecular imprinting magnetic microspheres

A technology of molecular imprinting and magnetic microspheres, applied in the fields of medicinal chemistry, organic chemistry and analytical chemistry, can solve the problems that have not yet been discovered, and achieve the effect of improving the difficulty of separation, good spheroidization, and not easy oxidation.

Inactive Publication Date: 2017-06-13
HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Through literature search at home and abroad, no related reports on the preparation of triphenanthridine alkaloid molecularly imprinted magnetic microspheres such as sanguinarine and chelerythrine have been found.

Method used

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  • Preparation method and application of benzophenanthridine alkaloid molecular imprinting magnetic microspheres
  • Preparation method and application of benzophenanthridine alkaloid molecular imprinting magnetic microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] 1. Fe 3 o 4 Nanoparticle preparation

[0045] 1.08g FeCl 3 ·6H 2 O was dispersed ultrasonically in 80ml of ethylene glycol. Then add 0.5 g of trisodium citrate and 1 g of PEG-2000 to the solution in sequence, and disperse by ultrasonic. Finally, 4.5 g of anhydrous sodium acetate were added. After the solution was stirred until it became clear and transparent, the solution was transferred to a 100ml reaction kettle and reacted at 200°C for 8h. After magnetic separation, wash three times alternately with water and absolute ethanol. After freeze-drying, Fe 3 o 4 nanoparticles.

[0046] 2. Fe 3 o 4 @SiO 2 Granule preparation

[0047] 0.25g Fe 3 o 4 The particles were added to the mixed solution of ethanol-water (160ml absolute ethanol / 40ml water), and ultrasonically dispersed for 30min. Transfer the obtained solution to a 250ml three-neck flask, stir at 500r / min for 15min, add 5ml of ammonia water, stir for 10min, then add 0.6ml of TEOS (tetraethyl orthosili...

Embodiment 2

[0053] 1. Fe 3 o 4 Nanoparticle preparation

[0054] 1.08g FeCl 3 ·6H 2 O was dispersed ultrasonically in 80ml of ethylene glycol. Subsequently, 0.5 g of trisodium citrate and 1 g of PEG-2000 were sequentially added to the solution, and ultrasonically dispersed. Finally, 4.5 g of anhydrous sodium acetate were added. After the solution was stirred until it became clear and transparent, the solution was transferred to a 100ml reaction kettle and reacted at 200°C for 8h. After magnetic separation, wash three times alternately with water and absolute ethanol. After freeze-drying, Fe 3 o 4 nanoparticles.

[0055] 2. Fe 3 o 4 @SiO 2 Granule preparation

[0056] 0.25g Fe 3 o 4 The particles were added to the mixed solution of ethanol-water (160ml absolute ethanol / 40ml water), and ultrasonically dispersed for 30min. Transfer the obtained solution to a 250ml three-neck flask, stir at 500r / min for 15min, add 5ml of ammonia water, stir for 10min, then add 0.6ml of TEOS (t...

example 3

[0062] 1. Preparation of Boluohui Extract

[0063] Take 200g of Boluohui fruit pods, extract by percolating with 5 times of 1% hydrochloric acid water at 90°C for 3 times, 1 hour each time. After solid-liquid separation, the filtrate was diluted 3 times and used as the extract for later use.

[0064] 2. Separation and purification of sanguinarine and chelerythrine in the extract

[0065] Add 10g of molecularly imprinted magnetically imprinted polymer microspheres on the surface of sanguinarine to the extract, shake fully for 30 minutes, let stand for 30 minutes, insert the extract with a strong magnet, and place the molecularly imprinted magnetically imprinted polymer microspheres on the surface of sanguinarine Adsorbed out, then put the microspheres in a chromatographic column with a diameter of 1cm, and continuously and slowly elute (wash) twice with 100ml of acidic methanol of 2% hydrochloric acid, then concentrate the eluent and recrystallize to obtain 98% of the Sanguin...

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Abstract

The invention relates to a preparation method and application of benzophenanthridine alkaloid (such as sanguinarine and chelerythrine) molecular imprinting magnetic polymer microspheres. The method comprises the steps of (1) preparing Fe3O4 nano-particles; (2) preparing Fe3O4@SiO2 particles; (3) Viny1- Fe3O4@SiO2 particles; (4) synthesizing a surface molecular imprinting magnetic polymer; and (5) separating and purifying two benzophenanthridine alkaloids (sanguinarine and chelerythrine) from a traditional Chinese medicine extract solution. The prepared benzophenanthridine alkaloid molecular imprinting magnetic polymer microspheres prepared according to the invention have good magnetism; specific separation of benzophenanthridine alkaloids can be achieved; the obtained alkaloids are high in purity, simple in operation, cheap and available in raw material and low in cost; and the method has a wide application prospect in the aspects of separation, enrichment and detection of the benzophenanthridine alkaloids and analogues thereof.

Description

technical field [0001] The present invention relates to the fields of medicinal chemistry, organic chemistry and analytical chemistry, in particular to the preparation of molecularly imprinted magnetic polymer microspheres (abbreviated) of benzophenanthridine alkaloids (such as sanguinarine, chelerythrine, etc.) method and application. Background technique [0002] Boluohui, Xiaoguoboluohui, Xueshuicao, celandine and other medicinal plants are rich in a variety of benzophenanthridine alkaloids (such as sanguinarine, chelerythrine, dihydrosanguinarine, Dihydrochelerythrine, oxidized sanguinarine, etc.), among which alkaloids such as sanguinarine and chelerythrine have attracted much attention due to their pharmacological activities such as antiviral, bactericidal, and anticancer. These alkaloids The separation and purification of alkaloids has always been a hot issue in the research of alkaloid drugs. The traditional separation methods of triphenanthridine alkaloids mainly ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/153C07D491/056C08F226/06C08F222/14C08J9/26
CPCC07D491/056C07D491/153C08F226/06C08J9/26C08J2201/0424C08J2339/08C08F222/102
Inventor 钟明龙睿卿王艳红
Owner HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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