Preparation method and application of polyethylenimine-modifed magnetic microspheres

A technology of polyethyleneimine and magnetic microspheres, applied in chemical instruments and methods, alkali metal oxides/hydroxides, inorganic chemistry, etc., can solve the problem of low adsorption capacity and achieve good stability and reproducibility Good, simple and effective preparation method

Inactive Publication Date: 2018-10-09
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problems existing in the prior art, the present invention provides a preparation method and application of polyethyleneimine-modified magnetic microspheres, which overcomes the problem of low adsorption capacity of pure magnetic materials in the prior art

Method used

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  • Preparation method and application of polyethylenimine-modifed magnetic microspheres
  • Preparation method and application of polyethylenimine-modifed magnetic microspheres
  • Preparation method and application of polyethylenimine-modifed magnetic microspheres

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Example 1: Fe 3 o 4 Preparation method of @PDA@PEI magnetic microspheres

[0028] (1) Fe 3 o 4 Preparation of Magnetic Nanoparticles

[0029] 2.7g FeCl 3 ·6H 2 O and 7.2g of anhydrous sodium acetate were uniformly dispersed in 80mL of ethylene glycol under ultrasonic, and placed under room temperature under magnetic stirring for 3 hours to make it fully mixed; then, 3.0g of polyethylene glycol was added to the above-mentioned yellow solution; After stirring evenly, transfer them to a stainless steel reaction kettle and seal it; react at 200°C for 10 hours. After cooling to room temperature, the product was washed three times with absolute ethanol and ultrapure water, and then dried under vacuum at 50°C for 2 hours.

[0030] (2) PDA-coated Fe 3 o 4 Preparation of magnetic nanoparticles (Fe 3 o 4 @PDA)

[0031] 180mg Fe 3 o 4 Nanoparticles were ultrasonically dispersed in 80.0mL of Tris-HCl solution (10mM, pH 8.5), and then 10.0mL of Tris-HCl solution in whi...

Embodiment 2

[0034] Embodiment 2: Structural characterization of magnetic materials

[0035] (1) Particle size and morphology characterization

[0036] The particle size and morphology of the prepared magnetic microspheres were observed by JEM100CXII transmission electron microscope (JEOL Corporation) and NOVA NanoSEM 430 (US FEI Company) field emission scanning electron microscope. from figure 1 It can be seen that the synthesized bare Fe 3 o 4 Nanoparticles are regular spherical, uniform particle size, and good dispersion; Fe 3 o 4 @PDA nanoparticles have an obvious core-shell structure, and the thickness of the PDA layer on its surface is about 20nm. figure 1 (c) is Fe 3 o 4 The scanning electron microscope image of @PDA@PEI, this result further proves that the functionalized magnetic nanoparticles have a regular spherical structure, and the particle size is uniform; A more serious reunion between them.

[0037] (2) Element characterization

[0038] The X-ray energy loss spect...

Embodiment 3

[0045] Example 3: The magnetic microspheres of surface-modified polyethyleneimine are used to determine four kinds of pigments in food

[0046] Under optimized experimental conditions, four mixed pigment standard solutions of a series of concentrations were prepared for liquid chromatography separation (instrument model was 1260 high performance liquid chromatography (Agilent Technologies (China) Co., Ltd.); the chromatographic column was Venusil XBPC 18 Column (150×4.6mm i.d., 5μm), the column temperature was constant at 30°C; the mobile phase was 20mM ammonium acetate-methanol, the flow rate was 1mL / min, and the injection volume was 20μL), and the peak area of ​​each analyte was compared with the concentration. Calibrate the curve, and use the least square method to perform linear regression at the same time, the results are shown in Table 1, the linear range of the four pigments is wide, and they have good correlation, and the correlation coefficient is greater than 0.999. ...

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Abstract

The invention discloses a preparation method and application of polyethylenimine-modifed magnetic microspheres. The preparation method comprises the following steps: firstly synthesizing ferroferric oxide magnetic microspheres, then performing ultrasonic dispersion on the prepared Fe3O4 nanoparticles in a Tris-HCI solution and then dropwise adding a dopamine-dissolved Tris-HCl solution; reacting under the action of mechanical stirring and drying to obtain dry Fe3O4@PEI magnetic microspheres; finally dispersing the prepared Fe3O4@PEI nanoparticles in the Tris-HCI solution, slowly adding a PEI aqueous solution, reacting under water bath conditions and drying to obtain the dry Fe3O4@PDA@PEI magnetic microspheres. The preparation method disclosed by the invention is simple, effective and goodin reproducibility; the prepared magnetic microspheres are uniform in particle size, larger in specific area, controllable in size, quick in response to an external magnetic field, good in selectivity, capable of producing an electrostatic effect with a negatively-charged sulfonic acid group in a pigment, easy for pigment absorption, good in stability, renewable and reusable.

Description

technical field [0001] The invention belongs to the technical field of functional materials and analysis, and in particular relates to a surface-modified polyethyleneimine Fe 3 o 4 The preparation method of magnetic microspheres and its application in the determination of four pigments of amaranth, carmine, sunset yellow and allura red in food. Background technique [0002] In the process of analysis and detection, since complex sample systems such as food, environment and biology are mostly mixtures of many different substances, and the content of target compounds is often very low, they cannot be directly detected by instruments. Therefore, effective pretreatment methods for samples, For example, separation, purification and enrichment are the prerequisites for accurate analysis and identification. Currently commonly used sample pretreatment techniques include liquid-liquid extraction and solid-phase extraction. However, traditional solid-phase extraction and liquid-liq...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/28B01J20/30G01N30/02
CPCB01J20/28009B01J20/28021B01J20/286G01N30/02
Inventor 丁国生陈惠邓小娟
Owner TIANJIN UNIV
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