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Preparation method and application of ochratoxin metal organic skeleton-molecular imprinting compounded separation medium

A metal-organic framework and ochratoxin technology, applied in chemical instruments and methods, and other chemical processes, can solve the problems of high price, easy to be affected by sample matrix, pH, solvent, salt concentration, etc., and low extraction efficiency

Active Publication Date: 2017-09-01
HENAN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] For trace amounts of ochratoxins in complex matrices, traditional liquid-liquid solvent extraction for sample pretreatment is inefficient, and the purification effect of commercial immunoaffinity columns is easily affected by sample matrix, pH, solvent, salt concentration, etc. At the same time, it is expensive and difficult to reuse. The present invention uses a metal organic framework as a carrier and adopts a precipitation polymerization method to synthesize a metal organic framework-molecularly imprinted composite. The technical problem to be solved is to provide a complex matrix. Preparation method of metal-organic framework-molecularly imprinted complex with specific molecular recognition ability of ochratoxin

Method used

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  • Preparation method and application of ochratoxin metal organic skeleton-molecular imprinting compounded separation medium
  • Preparation method and application of ochratoxin metal organic skeleton-molecular imprinting compounded separation medium
  • Preparation method and application of ochratoxin metal organic skeleton-molecular imprinting compounded separation medium

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Experimental program
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Effect test

Embodiment 1

[0025] Add 1.0 mmol of 1-hydroxy-4-p-tolylaminoanthraquinone into a three-neck flask of absolute ethanol containing 1.5 g of activated metal-organic frameworks, 150 mL, and then add 5.0 mmol of butyl methacrylate, 30 mmol of ethylene glycol dimethyl Acrylate and 2.5% initiator azobisisobutyronitrile, ultrasonicated for 5 minutes, until the solution was evenly mixed, mechanically stirred (rotating speed 200 r min -1 ), placed in a constant-temperature oil bath at 75°C, reacted for 5 hours, raised to 90°C and matured for 1 hour, then sucked and dried to obtain an organic framework-molecularly imprinted complex containing a substitute template. The complex was washed with methanol / acetic acid (4:1, v / v) and methanol until no template molecules were washed out. After air-drying, vacuum-dry at 40°C for 48 hours to obtain an organic framework-molecular imprinted complex.

Embodiment 2

[0027] Add 1.0 mmol 1-hydroxy-4-p-tolylaminoanthraquinone to a 150 mL three-neck flask of absolute ethanol containing 1.5 g of activated metal-organic framework, then add 7.0 mmol butyl methacrylate, 30 mmol ethylene glycol dimethyl Acrylic acid ester and 2.5% initiator azobisisobutyronitrile, ultrasonic 5min, until the solution is mixed evenly, mechanical stirring (speed 200 r min -1 ), placed in a constant-temperature oil bath at 75°C, reacted for 5 hours, raised to 90°C and matured for 1 hour, and then filtered and dried to obtain an organic framework-molecularly imprinted complex containing a substitute template. The complex was washed with methanol / acetic acid (4:1, v / v) and methanol until no template molecules were washed out. After air-drying, vacuum-dry at 40°C for 48 hours to obtain an organic framework-molecular imprinted complex.

Embodiment 3

[0029] Add 1.0 mmol of 1-hydroxy-4-p-tolylaminoanthraquinone into a 150 mL three-neck flask of absolute ethanol containing 1.5 g of the activated metal-organic framework, then add 7.0 mmol of butyl methacrylate and 15 mmol of ethylene glycol Dimethacrylate and 2.5% initiator azobisisobutyronitrile, ultrasonicated for 5 minutes, until the solution was evenly mixed, mechanically stirred (rotating speed 200 r min -1 ), placed in a constant-temperature oil bath at 75°C, reacted for 5 hours, raised to 90°C and matured for 1 hour, and then filtered and dried to obtain an organic framework-molecularly imprinted complex containing a substitute template. The complex was washed with methanol / acetic acid (4:1, v / v) and methanol until no template molecules were washed out. After air-drying, vacuum-dry at 40°C for 48 hours to obtain an organic framework-molecular imprinted complex.

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Abstract

The invention relates to the technical field of separation medium preparation, in particular to a preparation method and application of an ochratoxin metal organic skeleton-molecular imprinting compounded separation medium. The ochratoxin metal organic skeleton-molecular imprinting compounded separation medium is taken as a filing material for a solid phase extraction column for being applied in selective enrichment and separation of the ochratoxin in complex matrix. A imprinted polymer takes a structural analogue of the ochratoxin as an alternative template, and a metal organic skeleton is combined with the imprinted polymer to prepare the ochratoxin metal organic skeleton-molecular imprinting compounded separation medium. The separation medium prepared by the invention has the porosity characteristic of the metal organic skeleton and the molecular recognition ability of the molecular imprinting polymer to a target molecule, can selectively enrich and isolate the ochratoxin, is applied to the sample pretreatment of the complex matrix to achieve better purification, enrichment effect, and has broad application prospects.

Description

technical field [0001] The invention belongs to the technical field of food safety analysis and detection, and in particular relates to a method for preparing a metal-organic framework-imprinted polymer with specific molecular recognition ability for ochratoxin in a complex matrix and its application. Background technique [0002] Ochratoxin is mainly produced by Aspergillus and Penicillium strains and is teratogenic, embryotoxic, genotoxic, neurotoxic, immunosuppressive, carcinogenic, and nephrotoxic, and more seriously, it can leave the host It persists under fungal conditions and has a long half-life of up to 35 days in humans. Therefore, ochratoxin has attracted widespread attention worldwide, and the International Agency for Research on Cancer has listed ochratoxin as a possible carcinogen (category 2B). [0003] The latest national standard in 2011 stipulates that the maximum limit of ochratoxin A in grains and their products is 5 μg kg -1 . It can be seen that the ...

Claims

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Application Information

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IPC IPC(8): C08G83/00C08F222/14C08F220/18C08J9/26B01J20/26B01J20/30
CPCB01J20/261B01J2220/4806B01J2220/4812C08F222/1006C08F222/102C08G83/008C08J9/26C08J2201/0424C08J2335/02C08F220/1804
Inventor 何娟许红宋立新吴超钧李媛媛张书胜
Owner HENAN UNIVERSITY OF TECHNOLOGY
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