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Liquid-liquid interface detection method for surface-enhanced Raman spectroscopy

A surface-enhanced Raman and detection method technology, applied in the field of sensitive analysis and detection, can solve the problems of non-transplantation, time-consuming, susceptible to interference, etc., to reduce the influence of background signals, improve throughput and efficiency, and ensure stable control Effect

Inactive Publication Date: 2018-07-06
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the complex structure and high cost of the micro-nano processing equipment used, the time-consuming and high-cost fabrication process, and the difficulty in mass production limit the wide application of this type of SERS active substrate.
Common substrate materials are also rigid materials such as porous alumina, silicon wafers or glass slides, however these are usually not portable and not suitable for complex surface analysis in the field
[0003] Using SERS as a quantitative detection technique is still a big challenge, because SERS is essentially a near-field phenomenon, and only molecules located at hot spots can be detected. In addition, the field enhancement at hot spots is closely related to the local structure and the coupling between them, so even though the molecules can be evenly distributed on the metal surface, the SERS signal may still be inhomogeneous
For the solid-gas interface, sensitivity and reproducibility are two irreconcilable indicators. The use of internal standards can solve the above problems. However, in the same physical and chemical environment, the positioning of internal standards and target molecules has the following problems: The standard molecule will compete for the adsorption site to replace the target molecule; the second is that the microenvironment will affect the stability of the signal of the internal standard molecule, resulting in changes and fluctuations in intensity
This method cannot guarantee the continuity and regularity of the assembled membrane, and has disadvantages such as insufficient rapidity, susceptibility to interference, and low consistency of large-scale assembly.
In Au@SiO 2 Adding ethanol to the two-phase system of particle sol and n-hexane induces the self-assembly of nanoparticles. This method has obvious shortcomings: the treatment of noble metal particles is cumbersome; more assembly volume is required; the rapid addition of ethanol will affect the flatness of the assembled film sexual density

Method used

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  • Liquid-liquid interface detection method for surface-enhanced Raman spectroscopy
  • Liquid-liquid interface detection method for surface-enhanced Raman spectroscopy
  • Liquid-liquid interface detection method for surface-enhanced Raman spectroscopy

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Gold particles were synthesized by citrate reduction method and hydroxylamine hydrochloride reduction method, and dispersed in the water phase after centrifugal concentration to form gold nano-sol;

[0035] After the apples are cleaned, remove the peel with a radius of 0.45 cm, drop 50 μL of thiram double standard solution, and let it dry naturally; extracted extract;

[0036] Take 50 μL of the extract and add it to 100 μL of gold nanosol. Under the induction of acetone, the gold nanoparticles self-assemble on the liquid-liquid interface into a nanoparticle array film with metallic luster (such as figure 1 shown), use it as a Raman scattering active substrate to directly detect Raman with a Raman spectrometer, the parameters of the Raman spectrometer: microscope objective lens × 20, excitation wavelength 785nm, detection wavelength 800-1600cm -1 , laser power 2mW, integration time 8s, accumulation times 1 time.

[0037] Such as figure 2 Shown in A is that the double...

Embodiment 2

[0040] Gold particles were synthesized by citrate reduction method and hydroxylamine hydrochloride reduction method, and dispersed in the water phase after centrifugal concentration to form gold nano-sol;

[0041] After cleaning the pears, remove the pericarp with a radius of 0.45 cm, add 50 μL of thiram double standard solution dropwise, and let it dry naturally; put it into a mixed solution of 450 μL of acetone and cyclohexane (10:1 by volume) Extraction; then take 50 μL of the extract and add it to 100 μL of gold nanosol. Under the induction of acetone, the gold nanoparticles self-assemble on the liquid-liquid interface to form a nanoparticle array film with metallic luster, which is used as a Raman scattering active substrate. Use a Raman spectrometer to directly perform Raman detection. The parameters of the Raman spectrometer: microscope objective lens × 20, excitation wavelength 785nm, detection wavelength 800-1600cm -1 , laser power 2mW, integration time 8s, accumulati...

Embodiment 3

[0045] The total molar number of the two analytes, thiram and tiramidine, is 1.25×10 -10 mol, the molar ratios of the two are 5:0, 4:1, 3:2, 2:3, 1:4, 0:5, respectively.

[0046] The detection system is 100 μL of gold nanoparticle sol and 50 μL of cyclohexane and acetone (v:v=1:1) containing the analyte, both of which are dissolved in the organic phase; -1 、1010cm -1 The characteristic peaks are respectively used as the linear indicators of thiram and Tibiline two analytes. The parameters of the Raman spectrometer are: microscope objective lens × 20, excitation wavelength 785nm, detection wavelength 400-1600cm -1 , laser power 2mW, integration time 8s, accumulation times 1 time.

[0047] Figure 4 A is the Raman spectrum of the two pesticides with different molar ratios. It shows that the Raman intensity increases linearly with the increase of the molar number of Albiline; at the same time, the Raman intensity decreases gradually with the decrease of the molar number of th...

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Abstract

The invention provides a liquid-liquid interface detection method for surface-enhanced Raman spectroscopy. The method comprises: first, preparing an oil phase solution containing acetone and noble metal nano sol respectively; dissolving a to-be-detected substance in the oil phase solution or noble metal nano sol; then mixing the oil phase solution and the noble metal nano sol to form a liquid-liquid two-phase interface; and finally, detecting target molecules in the to-be-detected substance by a Raman spectrometer by utilizing a noble metal nano-particle array self-assembled on the liquid-liquid interface as an active substrate for Raman scattering. The method provided by the invention uses an insoluble liquid-liquid two-phase interface self-assembled noble metal nano-particle array as theRaman scattering active substrate for detection, can be used for single-phase or two-phase, single-component or multi-component detection of water-soluble / oil-soluble substances to be detected, breaks the bottleneck of detection of substances to be detected with different solubility in complex samples, and realizes high-throughput quantitative detection.

Description

technical field [0001] The invention relates to the field of sensitive analysis and detection, in particular to a liquid-liquid interface detection method with high reproducibility, ultra-stable and rapid surface-enhanced Raman spectroscopy. Background technique [0002] Surface-enhanced Raman scattering (SERS) is based on the special nano-size effect exhibited by noble metal nanoparticles, which solves the problem of weak conventional Raman scattering signals and achieves ultra-high sensitivity detection. Therefore, it is widely used in the fields of life science, environmental biology and public food safety. At present, the commonly used SERS substrate is in the state of colloidal solution, by adding anion (such as Cl - 、Br - etc.) to promote the agglomeration of nanoparticles in the solution, so that these agglomerated or complex-structured noble metal nanoparticles tend to generate more hot spots. However, the agglomeration phenomenon is uncontrollable and random, res...

Claims

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Application Information

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IPC IPC(8): G01N21/65
CPCG01N21/658
Inventor 刘洪林于烦烦苏梦可田丽
Owner HEFEI UNIV OF TECH
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