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Method for preparing molecular imprinting solid-phase extraction column of coumarin rodenticide

A solid-phase extraction column, molecular imprinting technology, applied in chemical instruments and methods, other chemical processes, etc., to achieve the effects of high enrichment multiples, simple preparation process, and strong specificity and selectivity

Inactive Publication Date: 2014-03-26
NINGBO MUNICIPAL CENT FOR DISEASE CONTROL & PREVENTION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method of the molecularly imprinted solid-phase extraction column about coumarin rodenticides has not been reported yet

Method used

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  • Method for preparing molecular imprinting solid-phase extraction column of coumarin rodenticide
  • Method for preparing molecular imprinting solid-phase extraction column of coumarin rodenticide
  • Method for preparing molecular imprinting solid-phase extraction column of coumarin rodenticide

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preparation example Construction

[0012] The preparation method of the coumarin rodenticide molecularly imprinted solid-phase extraction column of the present invention comprises the following steps:

[0013] 1. Mix 100~500mg of coumarin rodenticide molecularly imprinted polymer with 5~20mL of pure organic solvent, shake for 5~30min, ultrasonicate for 5~30min until the mixture is uniform, and transfer to the solid phase extraction of polypropylene and other materials In the small column, after the filling is uniform, both ends are respectively sealed with sieve plates.

[0014] The coumarin-type rodenticide molecularly imprinted polymer is preferably in powder form.

[0015] Molecularly imprinted polymers of coumarin rodenticides can be prepared by the following steps:

[0016] (1) Preparation of monodisperse polymer composite microspheres rich in epoxy groups: under the condition of 80°C, polymerized monomers, functional monomers and crosslinking agents were prepared by suspension polymerization reaction und...

Embodiment 1

[0032] Preparation of molecularly imprinted solid-phase extraction column for coumarin rodenticides:

[0033] (1) Mix 100 mg of coumarin rodenticide molecularly imprinted polymer with 10 mL of pure organic solvent, oscillate for 10 min, then sonicate for 10 min until the mixture is uniform, transfer to a solid-phase extraction column made of polypropylene or other materials, and use Sieve plate plugging;

[0034] (2) Mix 500mg of traditional solid-phase extraction filler with 10mL of pure organic solvent, oscillate for 10 minutes and then sonicate for 10 minutes to mix evenly, then transfer to the solid-phase extraction column obtained in step (1), fill it evenly and seal the top with a sieve plate, Wash the column with 10mL of acidic organic solvent, and then wash with 10mL of pure organic solvent to remove acidic substances;

[0035] (3) The solid-phase extraction obtained in step (2) was purged with an inert gas to remove the residual organic solvent, and vacuum-dried at 3...

Embodiment 9

[0051] Example 9: Preparation of Molecularly Imprinted Polymers of Coumarin Rodenticides

[0052] 1. Weigh 2.0g of polyvinyl alcohol 217 in 500.0mL of ultrapure water, heat to dissolve, and use it as a dispersant; polymerize monomer methyl methacrylate (4.0mL), functional monomer glycidyl methacrylate Ester (4.0mL) and cross-linking agent divinylbenzene (2.0mL) were successively added dropwise to the reaction system under stirring, and ultrasonically dispersed at 60°C for 5.0 minutes to make the reaction system evenly dispersed. Dissolve 1.0g of permethoxybenzoyl permethoxybenzoyl initiator in 20.0mL of hot ethanol solution, add it dropwise to the above reaction system at 80°C and 800 rpm, react at constant temperature and speed for 3.0 hours, successively use Washed several times with ultrapure water and ethanol, and vacuum dried at 60°C for 12 hours to prepare epoxy-functionalized polymer composite microspheres.

[0053] 2. Weigh 2.0g of template molecules and 10.0mL of ami...

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Abstract

The invention discloses a method for preparing a molecular imprinting solid-phase extraction column of a coumarin rodenticide. The method comprises the following steps of: sequentially uniformly mixing 100-500mg of imprinting polymers of the coumarin rodenticide, 100-500mg of traditional solid-phase extraction fillers and 5-20mL of pure organic solvent, sequentially transferring a mixture into a hollow solid-phase extraction column, blocking two ends of the hollow solid-phase extraction column through sieve plates, cleaning by an acidic organic solvent upper column after uniformly filling, flushing by the pure organic solvent, sweeping by inert gas to remove residual organic solvent, and drying to obtain the molecular imprinting solid-phase extraction column of the coumarin rodenticide. The method for preparing the molecular imprinting solid-phase extraction column of the coumarin rodenticide, disclosed by the invention, is simple and has specificity matching the self molecular imprinting polymer of the coumarin rodenticide, and the prepared solid-phase extraction column has higher selectivity and recovery rate on the coumarin rodenticide and can remarkably reduce matrix effect.

Description

technical field [0001] The invention relates to a preparation method of a solid phase extraction column, in particular to a preparation method of a coumarin rodenticide molecularly imprinted solid phase extraction column. Background technique [0002] In recent years, coumarin rodenticides [such as: chlorowarfarin (3-(α-p-chlorophenyl-β-acetylethyl)-4-hydroxycoumarin), warfarin (3-( 1-acetonylbenzyl)-4-hydroxycoumarin)] as the first generation of anticoagulant rodenticide, because of its high efficiency, broad spectrum, good palatability, etc., it is still the field and indoor rodenticide. main rat poison. However, due to the imperfect use and management, adults and children accidentally ingest, commit suicide, take poison and poisoning cases often occur. In view of this, the research on the enrichment, purification and detection technology of trace coumarin rodenticides is conducive to the advancement of sanitary inspection technology. [0003] For the detection of couma...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/30B01J20/26B01J20/285
Inventor 金米聪陈晓红赵永纲
Owner NINGBO MUNICIPAL CENT FOR DISEASE CONTROL & PREVENTION