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Antibiotic Raman spectrum detection method based on surface-modified magnetic nano-silver flower substrate

A Raman spectroscopic detection and magnetic nanotechnology, applied in Raman scattering, measurement devices, material analysis by optical means, etc., can solve the problems of cumbersome processing, time-consuming, labor-intensive, etc.

Inactive Publication Date: 2017-10-24
ACADEMY OF MILITARY MEDICAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These methods have high sensitivity, good repeatability, and are widely used, but they require professional personnel to operate, and the sample pretreatment process is cumbersome, time-consuming, and labor-intensive.

Method used

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  • Antibiotic Raman spectrum detection method based on surface-modified magnetic nano-silver flower substrate
  • Antibiotic Raman spectrum detection method based on surface-modified magnetic nano-silver flower substrate
  • Antibiotic Raman spectrum detection method based on surface-modified magnetic nano-silver flower substrate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Preparation of a high-performance surface-modified magnetic nano silver flower:

[0034] figure 1 A schematic flow chart of the magnetic silver silver flower modified by n-hexanethiol is given. Its specific preparation method is divided into the following five steps: the first step is to coat a layer of SiO2 on the outside of 200nm Fe3O4 nanoparticles; the second step is to grow silver seed particles by chemical plating; the third step is to formaldehyde and ammonia in ultrasonic Under the conditions, the flower-like shell is rapidly reduced; the fourth step is that n-hexanethiol (C6) is connected to the Ag shell through a sulfhydryl group (-SH), and is combined with a chemical bond, relying on the self-assembled hydrophobic layer on the surface of the magnetic nano silver flower and the antibiotic molecule. The hydrophobic interaction enriches the antibiotic molecules; the fifth step is to wash the SERS substrate (Fe3O4@SiO2-Ag-C6) modified by n-hexanethiol (C6) with ...

Embodiment 2

[0037] Antibiotic Raman spectroscopy detection method based on surface-modified magnetic nano silver flower substrate was used for qualitative and quantitative analysis of two antibiotic solutions:

[0038] image 3 It is the result of qualitative and quantitative analysis of chloramphenicol solution. Using Fe3O4@SiO2-Ag-C6 SERS substrate for concentrations ranging from 10 -3 ~10 -10 The chloramphenicol solution of M was detected by Raman, and the 80% ethanol used to prepare the chloramphenicol solution was used as a signal reference, and the obtained SERS spectrum was as follows image 3 As shown in A. The SERS signal intensity gradually decreased with the decrease of chloramphenicol concentration. Since the SERS signal intensity is very sensitive to the concentration of chloramphenicol, the background-subtracted SERS signal intensity of chloramphenicol was used to plot its concentration. image 3 a is chloramphenicol at 1347cm -1 The log-log relationship between the inte...

Embodiment 3

[0041] Figure 5-Figure 7 It is the qualitative and quantitative analysis results of chloramphenicol in milk and ciprofloxacin in milk. Taking blank milk as a signal reference, the obtained SERS spectrum is as follows: Figure 5 A. Image 6 Shown in B. Such as Figure 5 a, Image 6 As shown in b, we have selected the characteristic peak 1347cm of chloramphenicol in the spectrogram -1 , the characteristic peak of ciprofloxacin is 1387cm -1 , plotted their log-log curves according to their solution concentrations and corresponding characteristic peak intensities. Chloramphenicol, ciprofloxacin in 10 -3 ~10 -9 Within the concentration range of M, obtain the linear equation y=6818+653.05879x, r respectively 2 =0.99; y=13843+1212.5468x, r 2 =0.98, the linear relationship is good. The detection limits of this method to chloramphenicol and ciprofloxacin in milk are respectively 0.1nM (30ppt), 1nM (331ppt), far below the maximum residue 0.3ng / mL (300ppt) stipulated in the 2...

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Abstract

The invention discloses an antibiotic Raman spectrum detection method based on a surface-modified magnetic nano-silver flower substrate. The detection method comprises the following steps: coating Fe3O4 nanoparticles of 200nm with a SiO2 layer, generating a large amount of silver seeds on the surface of the SiO2 shell, and breeding a flower-shaped structure by taking seeds as a core; connecting 1-hexanethiol with Ag shell through a sulfhydryl group, and enriching antibiotics by using a surface self-organization hydrophobic layer; diluting the two kinds of antibiotics respectively with methanol water and milk to different concentrations, and purifying and enriching with a SPE (Solid-Phase Extraction) column; acquiring lowest detection limits of the antibiotics in different substances through the Raman spectrum detection, wherein a standard recovery rate is between 78.50 and 113.59 percent. The method is high in recovery rate, and can satisfy the requirement on antibiotics residue analysis. The 1-hexanethiol-modified magnetic nano-silver flower particles prepared by the invention are taken as a high-performance the SERS (Surface Enhanced Raman Scattering) substrate, are provided with a large quantity of hot spots, and can be taken as simple, rapid, high-sensitivity antibiotics residue analysis method.

Description

technical field [0001] The invention relates to the preparation of a surface-modified magnetic nano silver flower SERS substrate, in particular to an antibiotic Raman spectrum detection method based on the surface-modified magnetic nano silver flower substrate, and belongs to the fields of photonic materials, nanomaterials and food safety detection. Background technique [0002] Food safety issues have attracted widespread attention from the international community, and antibiotic residues are an important part of food safety testing. At present, most of the traditional detection and analysis methods for antibiotics in food are high-performance liquid chromatography, gas chromatography, gas chromatography-mass spectrometry, liquid chromatography-mass spectrometry and other methods in the laboratory. These methods have high sensitivity, good repeatability, and are widely used, but they require professionals to operate, and the sample pretreatment process is cumbersome, time-c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65
CPCG01N21/658
Inventor 王升启李萍肖瑞汪崇文李敏荣振
Owner ACADEMY OF MILITARY MEDICAL SCI
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