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Novel method for determining thiocyanate ion content of actual sample

A technology of thiocyanate and ion content, applied in the direction of material excitation analysis, Raman scattering, etc., can solve the problems of difficult electrode preparation, easy fluorescence quenching, instability, etc., and achieve simple and fast operation, good optical stability, highly reliable effect

Active Publication Date: 2018-05-15
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] For SCN - At present, ion chromatography is mostly used for detection, but ion chromatography requires more complex sample pretreatment process and the established standard working curve has a narrow range, which limits the SCN in actual samples. - detection; high performance liquid chromatography, mass spectrometry, and gas chromatography-mass spectrometry generally require toxic reagents for a cumbersome sample pretreatment process, which inevitably produces a lot of waste, and the analysis process is time-consuming and requires professional operators; capillary electrophoresis and Electrochemical methods require chemically modified electrodes or ion-selective electrodes, but electrode preparation is difficult and easily interfered by halide ions; SCN established by atomic absorption spectroscopy and UV-visible absorption spectroscopy - detection, the sensitivity is poor, and fluorescence spectroscopy is easy to quench and unstable due to fluorescence

Method used

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  • Novel method for determining thiocyanate ion content of actual sample
  • Novel method for determining thiocyanate ion content of actual sample
  • Novel method for determining thiocyanate ion content of actual sample

Examples

Experimental program
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preparation example Construction

[0028] Preparation of SERS active nanoprobe Au@Ag:

[0029] In this experiment, the signal molecule with a sulfhydryl internal standard designed and synthesized in the laboratory (see Chinese patent 201610351941.9 for details) was self-assembled on the surface of a gold nano-sol of about 20-30 nm through S-Au, and silver with better SERS effect was selected as the packaging material for packaging. Au@Ag nanoprobes with SERS activity were prepared on the surface of the enhanced substrate with the above-mentioned modified signal molecules.

Embodiment 1

[0032] The SERS nano-active probe Au@Ag prepared above was placed for different time, and Raman detection was performed respectively, 2208cm -1 There is no obvious change in the signal intensity at the position, and the nanoprobe has good stability, such as figure 1 shown.

Embodiment 2

[0034] Prepare 11 different concentrations of SCN - For the standard solution, take 240 μL of the SERS nanoprobe Au@Ag, and 250 μL of the above-mentioned different concentrations of SCN - The standard solution was mixed for 5 minutes, and the SCN - After the standard solution and the SERS nanoprobe Au@Ag were dispersed and balanced, 10 μL of 14 μM CTAB was added to the above mixture, and Raman detection was performed 5 minutes later. SCN - at 2110cm -1 The characteristic peak intensity at 2208cm and the internal standard signal -1 Compare the intensity of the characteristic peaks at the place, get the peak intensity ratio, and establish the SCN - The standard working curve of the concentration and peak intensity ratio; three months later, according to the above experimental operation, re-establish the working curve, and compare the two established standard working curves;

[0035] as attached figure 2 As shown, the left figure in the figure is the corresponding SERS spe...

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Abstract

The invention discloses a novel method for determining the thiocyanate ion content of an actual sample. The method comprises the following steps: using a signal molecule with the Raman scattering peakof 2208 cm<-1> wave number, selecting gold with appropriate size as a reinforcement substrate of a Raman signal, self-assembling the signal molecule onto the surface of the reinforcement substrate, and then selecting silver with a relatively good SERS effect as an enveloping shell layer for probe encapsulation; comparing the characteristic peak intensity of thiocyanate ions at 2110 cm<-1> with the characteristic peak intensity of the signal molecule at 2208 cm<-1>, and drawing a standard working curve according to the molar concentration and the peak intensity ratio of the thiocyanate ions; mixing an SERS nanoprobe and a solution to be detected, standing for 5 minutes, adding CTAB into the mixed solution after the solution to be detected and the SERS nanoprobe are dispersed in a balancedway, measuring the characteristic peak intensity ratio of the thiocyanate to the signal molecule by using a Raman spectrometer 5 minutes later, and substituting the intensity ratio into the drawn standard working curve to determine the thiocyanate content of the actual sample.

Description

technical field [0001] The present invention relates to the preparation of a surface-enhanced Raman scattering (Surface-enhanced Raman scattering, SERS) active nano-labeled probe with a sulfhydryl group and a Raman signal located in a biological silent zone, and a method for the determination of sulfur in actual samples using the SERS method Method for cyanate content. Background technique [0002] Human body fluids (saliva, blood, urine) contain thiocyanate ions (SCN - ), mainly obtained through ingestion of Brassica vegetables, cheese and milk. SCN in human body - The increase in concentration will affect the secretion pathway of iodine in the thyroid gland, increase the risk of cancer, produce adverse cardiovascular risks, and affect the protein dialysis of the human body; as a typical halogen-like ion, SCN - With strong coordination ability and halogen properties, the SCN - Adding peroxides and peroxides to milk powder can block bacterial metabolism and have good ant...

Claims

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Application Information

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IPC IPC(8): G01N21/65
CPCG01N21/65
Inventor 沈爱国白向茹任家强胡继明
Owner WUHAN UNIV
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