Capillary micro-droplet metal ball detection method for surface enhanced Raman spectrum

A technology of surface-enhanced Raman and detection methods, applied in the field of sensitive detection and analysis, can solve the problems of large volume and difficult laser focusing, and achieve the effects of simple operation, real-time quantitative detection, and less spectral spurious peaks.

Active Publication Date: 2018-06-05
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method does not control the distance between the interfacial nanoparticles to optimize the enhanced strength of the electromagnetic field, and there are disadvantages such as the volume of the system required to collect signals in the cuvette is relatively large, and the laser is not easy to focus.

Method used

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  • Capillary micro-droplet metal ball detection method for surface enhanced Raman spectrum
  • Capillary micro-droplet metal ball detection method for surface enhanced Raman spectrum
  • Capillary micro-droplet metal ball detection method for surface enhanced Raman spectrum

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Experimental program
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Effect test

Embodiment 1

[0051] A method for detecting capillary micro-droplet metal balls for surface-enhanced Raman spectroscopy, the steps are as follows:

[0052] (1) Mix the noble metal nano-sol with an organic solvent with a density greater than water, and then add the extract of the analyte to shake vigorously;

[0053] (2) The noble metal nanomaterials in the noble metal nanosol are quickly assembled at the oil-water interface to form micro-droplet metal balls with adjustable gaps between nanomaterials;

[0054] Such as figure 1 The enlarged schematic diagram is shown, gold nanoparticles and analyte molecules are quickly assembled at the oil-water interface to form micro-droplet metal balls with adjustable gaps between nanomaterials;

[0055] (3) Utilize capillary action to suck the micro-droplet metal ball into the capillary;

[0056] (4) Place the above-mentioned capillary adsorbed with micro-droplet metal balls under a Raman spectrometer for detection, and the SERS characteristic fingerpr...

Embodiment 2

[0067] Add 30μL o-dichloroethane containing malachite green and 0.9mL gold particles with a diameter of 80nm (the enhancement effect of SERS is the best at this time) into the container vial treated with hydrophilicity, and shake vigorously to assemble into micro-droplet metal balls . Then transferred to the capillary for Raman detection, the concentration of malachite green was 1×10 -6 M, 5×10 -7 M, 1×10 -7 M, 5×10 -8 M, 1×10 -8 M, 5×10 -9 M , 1×10 -9 M and 0 M, such as image 3 shown. The Raman characteristic peaks of malachite green are: 436 cm -1 , 788cm -1 、896 cm -1 、1174 cm -1 、1367 cm -1 and 1616 cm -1 . Choose 1174 cm -1 The Raman peak at 656 cm -1 The o-dichloroethane peak at the place is used as the internal standard, and the result shows that when no internal standard is added, R 2 = 0.87753, R after internal standard treatment 2 = 0.98154. Raman parameters include: microscope objective lens × 20, excitation wavelength 785 nm, detection...

Embodiment 3

[0069] Crucian carp meat was crushed and homogenized, and then malachite green (MG) dissolved in o-dichloroethane was added to make malachite green concentrations of 0 M, 2.0×10 -8 M , 5.0×10 -8 M , 1.0×10 -7 M and 2.0×10 -7 M samples. Finally, an extract containing malachite green was prepared, and the preparation process was as follows: (1) Take 4.00±0.04g sample and mix with 1000μL of 9.5g / L hydroxylamine solution to prevent MG degradation, and react at room temperature for 15 minutes before extraction; (2) Add 2.0±0.2g anhydrous magnesium sulfate to the homogenate and vortex vigorously for 1 minute; (3) Add 4.0±0.1g aluminum oxide to the homogenate and vortex vigorously for 30 seconds to remove lipids in the sample; (4) Take the supernatant and put it in a centrifuge tube, and centrifuge at 15000rpm for 10 minutes. After centrifugation, transfer the supernatant to a 20mL test tube dried under nitrogen at 50°C, add 2.0±0.1g alumina, vortex for 30 seconds, then trans...

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Abstract

The invention provides a capillary micro-droplet metal ball detection method for a surface enhanced Raman spectrum. The method comprises the following steps: mixing noble metal nanometer sol and an organic solvent phase with the density greater than that of water, adding a to-be-detected object extracting liquid and performing severe oscillation; rapidly assembling the noble metal nanometer material on an oil-water interface to form micro-droplet metal balls with adjustable nanometer material gaps; absorbing the micro-droplet metal balls in the capillary by utilizing capillary action; puttingunder a Raman spectrometer and performing detection to acquire an SERS feature fingerprint signal of the to-be-detected object; correcting a Raman spectral signal of the to-be-detected object by taking feature peak of the organic solvent as internal standard. The method can be applied to single-phase or double-phase and single-component or multi-component detection of the water-soluble / oil-solubleto-be-detected object, the bottleneck of detection on the to-be-detected objects with different solubility in a complex sample is broken, an organic phase in an assembling system serves as internal standard and a square capillary are cleverly combined to realize quantitative detection, and the method is simple in manufacturing and convenient in operation.

Description

technical field [0001] The invention belongs to the field of sensitive detection and analysis, and in particular relates to a highly reproducible and ultra-stable capillary micro-droplet metal ball detection method for surface-enhanced Raman spectroscopy. Background technique [0002] Surface-enhanced Raman spectroscopy (SERS) is a highly sensitive analytical detection technique, which has been successfully applied to the detection of multiple analytes in complex systems due to its unique vibrational fingerprints and narrow spectral linewidth characteristics , even at the single-molecule level. However, traditional solid SERS substrates have some limitations that make SERS measurement challenging, such as (1) the non-uniformity of SERS signal: because SERS is essentially a near-field phenomenon, only molecules located at hot spots can be detected , and the field enhancement at the hot spot is related to the sensitive local structure of the molecules and the coupling betwe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65
CPCG01N21/658
Inventor 刘洪林苏梦可田丽于烦烦
Owner HEFEI UNIV OF TECH
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