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Preparation method of high-performance gold-shell magnetic microsphere and surface enhanced Raman scattering (SERS) application of high-performance gold-shell magnetic microsphere

A magnetic microsphere, high-performance technology, applied in the direction of microsphere preparation, magnetic materials, magnetic objects, etc., can solve the problems of uneven coating of gold shell, weak magnetic response ability, cumbersome preparation process, etc., to facilitate large-scale production , good repeatability and simple synthesis steps

Inactive Publication Date: 2017-08-01
ACADEMY OF MILITARY MEDICAL SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the existing problems of poor dispersion of gold-shelled magnetic microspheres, weak magnetic response ability, cumbersome preparation process, uneven coating of gold shells, etc., and to provide a simple synthesis, monodispersity, high magnetic response, structural Preparation method of uniform gold-shell magnetic microspheres, and as a high-performance magnetic SERS substrate for rapid detection of targets in solution

Method used

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  • Preparation method of high-performance gold-shell magnetic microsphere and surface enhanced Raman scattering (SERS) application of high-performance gold-shell magnetic microsphere
  • Preparation method of high-performance gold-shell magnetic microsphere and surface enhanced Raman scattering (SERS) application of high-performance gold-shell magnetic microsphere
  • Preparation method of high-performance gold-shell magnetic microsphere and surface enhanced Raman scattering (SERS) application of high-performance gold-shell magnetic microsphere

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Preparation of a high-performance gold-shell magnetic microsphere:

[0033] figure 1 A schematic diagram of the preparation process of high-performance gold-shell magnetic microspheres is given. Its specific preparation method is divided into the following four steps: the first step, adopts solvothermal synthesis method to synthesize Fe 3 o 4 Microspheres. 1.35 g of ferric chloride hexahydrate was dissolved in 40 ml of ethylene glycol, and magnetically stirred for 30 minutes. Then 2.7 g of anhydrous sodium acetate and 1 g of polyethylene glycol 8000 were added to the solution and stirred until the reactants were completely dissolved. Then, the mixture was transferred to a Teflon-lined autoclave (50 ml capacity) and heated to 200° C. for 8-48 hours. After the reaction, the product was collected magnetically, washed three times with deionized water and ethanol respectively, and finally the product was vacuum-dried at 60°C for 6 hours to obtain Fe 3 o 4 The microsph...

Embodiment 2

[0041] SERS performance characterization of high-performance gold-shell magnetic microspheres:

[0042] The commonly used Raman molecule p-mercaptobenzoic acid (PATP) was used to characterize the SERS performance of gold-shell magnetic microspheres. PATP has a sulfhydryl group, which will produce significant Raman characteristic peaks when combined with gold or silver. First configure different concentrations of PATP solutions (10 -5 -10 -11 M / L), then put into the synthesized gold-shell magnetic microspheres and mix and shake for 30 minutes, after magnetic separation, disperse the gold-shell magnetic microsphere concentrate on a clean silicon wafer, and perform Raman detection after drying.

[0043] Figure 5 It is the experimental result of Example 2. exist Figure 5 The middle abscissa is the Raman shift. Figure 5 The middle curve from top to bottom is the PATP Raman spectrum excited by high concentration to low concentration PATP adsorbed on gold-shell magnetic bead...

Embodiment 3

[0045] Vancomycin-modified high-performance gold-shell magnetic microspheres detect Escherichia coli in solution:

[0046] The peptide antibiotic vancomycin interacts with bacterial cell walls to form hydrogen bonds (both gram-positive and gram-negative bacteria are acceptable), so vancomycin-modified magnetic beads can capture various bacteria in solution. We put vancomycin-modified gold-shell magnetic microspheres into solutions containing different concentrations of Escherichia coli, mixed them and incubated them with shaking for 20 minutes, so that the gold-shell magnetic beads could fully capture Escherichia coli. Perform SERS detection. Figure 6 Schematic diagram of the enrichment and detection of bacteria for vancomycin-modified gold-shell magnetic microspheres.

[0047] Figure 7 Be the transmission electron microscope observation result of embodiment 3, Figure 8 It is the experimental result of embodiment 3. From Figure 7 It can be seen that the gold-shell mag...

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Abstract

The invention discloses a preparation method of a high-performance gold-shell magnetic microsphere and surface enhanced Raman scattering (SERS) application of the high-performance gold-shell magnetic microsphere. A substrate uses a Fe3O4 microsphere of 100-1,000 nanometers as a core to provide magnetism, polymer polyethyleneimine (PEI) is used as a multi-functional sandwiched layer to improve the dispersibility of the magnetic microsphere and absorb gold seeds of 3-5 nanometers, and finally, a uniform and stable gold shell is prepared by a seed reduction method. The preparation method comprises the following steps of firstly, modifying Fe3O4 microsphere with the PEI to form a polymer protection layer, and absorbing the gold seeds of 3-5 nanometers by means of strong positive electricity of polyethyleneimine; secondly, rapidly reducing the uniform and stable gold shell under an ultrasonic condition by a seed growing method and by taking hydroxylamine hydrochloride as a reducing agent; thirdly, adding high-concentration povidone (PVP) to improve the dispersibility of particles; and finally, obtaining the high-performance gold-shell magnetic microsphere. The invention also discloses application of the gold-shell magnetic microsphere prepared by the method in SERS detection. The gold-shell magnetic microsphere is high in magnetic response, good in dispersibility and stable in structure, has excellent SERS performance and can be used for SERS detection and analysis on various pollutants, pesticide residue, pathogenic microorganism and the like in a solution.

Description

technical field [0001] The invention relates to the fields of preparation of magnetic functional materials and biochemical spectrum analysis, in particular to a preparation method of high-performance gold-shell magnetic microspheres and its application in SERS detection. Background technique [0002] Gold nanomaterials have excellent electrical conductivity, catalytic activity and unique optical properties, and have received extensive research and attention for a long time. Gold-shell magnetic micro / nanoparticles not only have the characteristics of rapid enrichment of samples by magnetic beads, simple and quick use, but also maintain the excellent performance of gold nanomaterials. It is a very promising multifunctional nanomaterial. [0003] Surface Enhanced Raman Scattering (SERS) is an important trace analysis detection method, and gold nanomaterials are widely used in the field of SERS detection as an effective SERS substrate material. Recently, some literatures have r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01F1/00H01F41/00B01J13/02G01N21/65
CPCH01F1/0054B01J13/02G01N21/658
Inventor 王升启肖瑞汪崇文李敏邵丽婷史鹏辉徐胜平郭晶贾小飞
Owner ACADEMY OF MILITARY MEDICAL SCI
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