Method for rapidly detecting nitrite by using surface enhanced Raman spectrum and application thereof

A surface-enhanced Raman and nitrite technology, applied in Raman scattering, material excitation analysis, etc., can solve the problems of tedious nitrite detection method, inconvenient on-site detection, time-consuming and other problems

Active Publication Date: 2013-03-27
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the shortcomings of traditional nitrite detection methods such as cumbersome process, time-consuming and inconvenient on-site detection

Method used

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  • Method for rapidly detecting nitrite by using surface enhanced Raman spectrum and application thereof
  • Method for rapidly detecting nitrite by using surface enhanced Raman spectrum and application thereof
  • Method for rapidly detecting nitrite by using surface enhanced Raman spectrum and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1 SERS rapid detection of nitrite in ham sausage

[0040] 1.1 Main instruments and reagents:

[0041] DeltaNu Inspector portable Raman instrument, electronic balance;

[0042] NO 2 - Standard solution: Accurately weigh 0.0150g of NaNO dried in an oven for 24 hours 2 , dissolved in ultrapure water and transferred to a 100mL volumetric flask, and diluted to the mark to prepare a concentration of 100mg L -1 NO 2 - Stock solution, add 1 drop of chloroform, store at 4°C, dilute to the required concentration before use; p-nitroaniline (0.3%, m / v): weigh 0.3g of p-nitroaniline, dissolve in 100mL hydrochloric acid solution ( 1mol L-1 ), after mixing, put it in a brown bottle and store it at 4°C; Preservation; Au / SiO 2 : Au NPs radius 55nm, SiO 2 Shell thickness 1-2nm. Potassium ferrocyanide solution (106g L -1 ): Weigh 10.6g potassium ferrocyanide, dissolve in water, and dilute to 100mL; zinc acetate solution (220g L -1 ): Weigh 22.0g of zinc acetate, first ...

Embodiment 2

[0053] Example 2SERS rapid detection of nitrite in soil

[0054] In this application, the main instruments and reagents used, the drawing of the standard curve and the determination of interfering ions are the same as in Example 1.

[0055] 2.1 Soil sample processing:

[0056] The soil samples were placed at room temperature for 24 hours to air-dry naturally, and the dried soil was ground with a mortar and sieved through a 0.45mm sieve. Weigh 5g of the sieved sample (accurate to 0.0001g), add 25mL sodium chloride solution (2mol L -1 ), ultrasonically extracted for 90 min, placed in a centrifuge at 4000 rpm for 5 min, the supernatant was collected, filtered through a 0.45 μm filter membrane, and set aside. For spiked soil sample analysis, dilute 500 µL to a concentration of 100 mg L -1 NO 2 - Add it to 5g of soil, mix well, leave it at room temperature for 2h before extracting, the concentration of the standard is 10μg g -1 .

[0057] 2.2 Determination of soil samples: ...

Embodiment 3

[0059] Example 3 Rapid detection of nitrite in saliva by SERS

[0060] In this application, the main instruments and reagents used, the drawing of the standard curve and the determination of interfering ions are the same as in Example 1.

[0061] 3.1 Processing of saliva samples:

[0062] Measure a certain volume of saliva and dilute it with water to obtain a saliva sample. Then use the saliva sample to prepare a spiked concentration of 1.00 mg L -1 spiked saliva samples.

[0063] 3.2 Determination of saliva samples:

[0064] Take 200 μL of saliva sample and spiked saliva sample, add 2 μL of p-nitroaniline and 2 μL of diphenylamine in sequence, mix well, and let stand for 5 minutes. Take an equal volume of the above reaction solution and Au / SiO 2 In the sample tube, mix evenly, and detect with DeltaNu Raman instrument, excitation wavelength: 785nm, scan time: 1s, read 1395cm -1 For the peak area at the Raman shift, substitute 1395cm -1 The peak area-nitrite content stan...

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Abstract

The invention relates to a method for rapidly detecting nitrite by using a surface enhanced Raman spectrum, and the application of the method. A Raman signal of the nitrite self is very weak, an SERS (surface enhanced Raman spectrum) signal is also weak, a coupling dye is generated by using nitrite ions and a diazonium-coupling reagent under an acid or weak alkaline condition, the SERS signal of the coupling dye is strong, and the qualitative and quantitative detection is carried out on the nitrite by indirectly measuring the amount of the coupling dye through the SERS. According to the method, Au / SiO2 is used as an SERS substrate material, and the stability of particles is improved by a silica shell layer, so that the result repeatability is good. The method is applicable to rapid detection of the nitrite in complex samples such as a food sample, an environment sample and a biological sample, and has the advantages of simplicity, rapidness (about five minutes), high selectivity, on-site detection applicability, convenience in popularization and use and the like.

Description

technical field [0001] The invention relates to a method for rapidly detecting nitrite by surface-enhanced Raman spectroscopy, in particular to a method for rapidly detecting nitrite by surface-enhanced Raman spectroscopy and its application, and is suitable for the determination of nitrite in complex samples such as food, environment, and biological samples. Background technique [0002] Nitrite is an intermediate in the nitrogen cycle in nature. It is unstable and widely exists in water, soil and various foods. According to research, nitrite itself is a highly toxic substance, and it is also a carcinogen. - Nitrosamines. Nitrosamines can also enter the fetus through the placenta and have a swollen effect on the fetus. [0003] Nitrite is a commonly used additive in meat processing. It has the functions of inhibiting Clostridium botulinum, coloring meat and enhancing flavor. At present, there is no ideal substitute. The reaction of nitrite with aromatic amine or benzylam...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65
Inventor 李攻科张凯歌胡玉玲
Owner SUN YAT SEN UNIV
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