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Preparation method of magnetic molecularly imprinted composite material of chiral rodenticide bromadiolone

A technology of magnetic molecular imprinting and composite materials, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of high selectivity of polymers without molecular imprinting, poor selectivity of bromadiolone, inconvenient solid-liquid separation, etc., to achieve Ideal purification effect, high selectivity, and simple preparation process

Inactive Publication Date: 2013-01-16
NINGBO MUNICIPAL CENT FOR DISEASE CONTROL & PREVENTION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, regarding the enrichment and purification of bromadiolone, literatures mainly use polymer resins such as GDX101, GDX201, GDX301, GDX403, GDX501, XAD-2 (Tan Jiayi, Jiang Zhaolin, Wu Yuhong. Journal of Analytical Science, 1999, 15, 229.) and mixed Oasis HLB solid-phase extraction cartridges (M.C Jin, X.H Chen, Y.Zhu.J.Chromatogr.A, 2007, 1155:57), etc., but these enrichment materials do not have the specific high selectivity of molecularly imprinted polymers, and enrich The collection ability is weak, so its application is limited to a certain extent
The existing preparation technology of bromadiolone molecularly imprinted polymer basically concentrates on materials such as non-magnetic polymers as carriers, such as: Chang Jing et al. (Chang Jing, He Ruiqiong, Zhu Jun, etc. Invention Patent, CN 102070753A) a molecularly imprinted polymer of anticoagulant rat drug Dalong and its application as a solid phase extraction agent; , fast solid-liquid separation, which limits the application of this type of material
As for the use of nano-ferric iron tetroxide as a carrier and the chiral mouse drug bromadiolone as a template molecule, a functionalized compound rich in amino groups is obtained by means of suspension polymerization, hydrogen bonding, ring-opening reaction, and functional modification. The preparation method of magnetic molecularly imprinted composite materials and its application in the pretreatment of biological samples have not been reported in the relevant literature

Method used

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  • Preparation method of magnetic molecularly imprinted composite material of chiral rodenticide bromadiolone
  • Preparation method of magnetic molecularly imprinted composite material of chiral rodenticide bromadiolone
  • Preparation method of magnetic molecularly imprinted composite material of chiral rodenticide bromadiolone

Examples

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preparation example Construction

[0021] The preparation method of the amino-modified molecularly imprinted material of the coumarin rodenticide of the present invention comprises the following steps:

[0022] 1. Preparation of monodisperse magnetic polymer microspheres rich in epoxy groups: monodisperse magnetic polymer microspheres with high epoxy functional group content were prepared by suspension polymerization.

[0023] This step is specifically as follows: sequentially weigh 0~5.0g of oleic acid-modified nano ferric oxide particles, measure 1.0~20.0mL of epoxy functionalized monomer, 2.0~10.0mL of polymerized monomer, 0~4.0mL of cross-linked and add it to 50.0~500.0mL dispersant, ultrasonically disperse at 60°C for 1.0~10.0 minutes; then add 0.5~5.0g initiator, at 60~90°C, the stirring speed is 300~900 rpm / min, mechanical stirring at constant temperature and constant speed, after reaction for 0.5~5.0 hours, wash with ethanol several times until the pH is 6~8, and vacuum dry at 30~90°C for 1~24 hours to...

Embodiment 1

[0032] (1) Weigh 2.0g of polyvinyl alcohol 217 in 500.0mL of ultrapure water, heat to dissolve, and use it as a dispersant; mix 2.0g of nanometer ferric oxide particles modified with oleic acid, polymerized monomer methyl methacrylate (4.0mL), functionalized monomer glycidyl methacrylate (4.0mL), and crosslinking agent divinylbenzene (2.0mL), were added to the reaction system in turn under stirring, and ultrasonically dispersed at 60°C for 5.0 minutes , so that the reaction system is uniformly dispersed. Dissolve 1.0g of permethoxybenzoyl permethoxybenzoyl initiator in 20.0mL of hot ethanol solution, add dropwise to the above reaction system at 80°C and 800 rpm, react at constant temperature and speed for 3.0 hours, successively Wash several times with ultrapure water and ethanol, and vacuum-dry at 60°C for 12 hours to prepare epoxy-functionalized magnetic polymer microspheres.

[0033] (2) Weigh 2.0g template molecule and 10.0mL amino functional reagent respectively, and add...

Embodiment 2-15

[0036] Its operating steps are the same as in Example 1, and the raw material, raw material formula and preparation condition parameters of Examples 1-15 are shown in Table 1.

[0037] Table 1: Raw material components and preparation parameters of Examples 1-15 of the present invention

[0038]

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Abstract

The invention discloses a preparation method of a magnetic molecularly imprinted composite material of chiral rodenticide bromadiolone. The preparation method comprises the following steps of: adding magnetic nanometer ferroferric oxide particle modified via oleic acid to a dispersing agent; adding polymerizing monomer, functional monomer and cross-linking agent; ultrasonically dispersing; adding an initiator; heating; agitating to react to obtain single dispersive polymer composite microsphere rich in epoxy groups; washing until pH (Potential Of Hydrogen) reaches 6 to 8; then drying; adding composite reacting liquid of bromadiolone and an amino functional agent; heating; agitating to react; magnetically separate; washing until the pH reaches 6 to 8; adding organic solvent; ultrasonically eluting to remove template molecule bromadiolone until no bromadiolone an be detected in the eluant through superfast efficient liquid chromatography-tandem mass spectrum; and then drying to obtain a target product. The preparation method disclosed by the invention has the characteristics of being simple in preparation technology, controllable in magnet content, and controllable in ratio of functional group and the like; a product is applicable to enriching, purifying, analyzing and detecting of bromadiolone residual in a biological sample; and the preparation method has a wide application prospect.

Description

technical field [0001] The invention relates to a preparation method of an amino functionalized magnetic molecular imprinting composite material with a core-shell structure, in particular to a preparation method of an amino functionalized magnetic molecular imprinting material of the chiral mouse drug bromadiolone. Background technique [0002] Bromadiolone [chemical name: 3-[3-(4-bromobiphenyl)-3-hydroxy-1-phenylpropyl]-4-hydroxycoumarin] is a second-generation anticoagulant rodenticide Anticoagulant, highly toxic to rodents, can kill a variety of pests once poisoned, and is effective for the first generation of anticoagulant-resistant pests. It has a good control effect on domestic rats and wild rats. The concentration of commonly used poisonous bait is 0.005%, the half-life of bromadiolone is 60 hours, and the incubation period of poisoning is long. The symptoms of poisoning will appear after at least 12-24 hours, and it takes 3-5 days for the poisoning to reach its peak...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F292/00C08F220/14C08F212/08C08F220/32C08F8/32C08J9/26B01J20/26B01J20/30B01J20/285
Inventor 陈晓红赵永纲金米聪
Owner NINGBO MUNICIPAL CENT FOR DISEASE CONTROL & PREVENTION
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