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Method for rapidly and accurately detecting zearalenone toxin in grains based on SERS (Surface Enhanced Raman Scattering)

A technology for zearalenone and toxin, which is applied in the preparation of test samples, measuring devices, instruments, etc., can solve the problems of complicated experimental pretreatment process and high detection cost, and achieves reduction of detection cost, low cost and time saving. and cost effects

Pending Publication Date: 2022-03-22
XIAMEN UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above methods are highly specialized and technical, the experimental pretreatment process is complicated, and the detection cost is high. Although some shortcomings of the traditional detection methods are made up for, it is necessary to develop a fast, accurate and low-cost detection method for practical application in food safety. method

Method used

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  • Method for rapidly and accurately detecting zearalenone toxin in grains based on SERS (Surface Enhanced Raman Scattering)
  • Method for rapidly and accurately detecting zearalenone toxin in grains based on SERS (Surface Enhanced Raman Scattering)
  • Method for rapidly and accurately detecting zearalenone toxin in grains based on SERS (Surface Enhanced Raman Scattering)

Examples

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Effect test

preparation example Construction

[0036] Preparation of Ag sol: The present invention adopts a one-pot method of Ag sol to enhance the Raman detection signal of ZEN azo reaction product. Ag sol was prepared by reducing AgNO with sodium citrate 3According to the method, Ag nanoparticles with particle size of 80-100nm were synthesized. First take 1mL of 0.1M AgNO 3 Add the solution to 100mL water, heat to boil, then add 2.5mL 1% sodium citrate solution, continue heating for 3 hours, and cool to room temperature to obtain Ag sol for later use. figure 1 It is a scanning electron microscope characterization diagram of Ag nanoparticles in Ag sol, and it can be seen that the Ag particles have a uniform diameter of 80-100nm.

[0037] Extraction of ZEN toxin: fully disperse and soak the grain sample to be tested in water, add extractant, the extractant is chloroform, ethyl acetate, dichloromethane, n-hexane, n-butanol, cyclohexane, methanol, acetonitrile and acetone One or several of them were vortexed for 0.5-2min,...

Embodiment 1

[0041] Collect the SERS curves of the products after the azo reaction between ZEN standard samples of different concentrations and the azo reaction solution: configure 10 standard solutions containing different concentrations of ZEN, respectively 0, 1, 10, 25, 50, 100, 250, 500 . -5 M and 200 μL of azo reaction auxiliary reagent (the mass fraction of sodium nitrite solution used is 1%, the mass fraction of sodium carbonate solution is 1%, and the volume ratio of sodium nitrite solution and sodium carbonate solution is 1:1). Nitrogen reaction, the reaction product is detected by SERS with the same volume of Ag sol, and the SERS spectrum of the product after the azo reaction of ZEN standard samples with different concentrations is obtained.

[0042] image 3 It is the SERS spectrum of the azo reaction product of the standard sample with a concentration of 50 μg / LZEN and the blank sample. It can be clearly seen from the figure that the spectrum of the blank sample is 1386cm -1 ...

Embodiment 2

[0046] In this example, ZEN standard substance was added to wheat flour without ZEN toxin, and the addition amounts were 60 μg / kg, 300 μg / kg, and 600 μg / kg respectively, and 1 g of the grain samples to be tested were fully dispersed and soaked in water, and 5 mL was added to extract acetonitrile, vortex and mix for 1min, then add 3g of buffer salt and cleaning agent, buffer salt and cleaning agent are MgSO 4 , NaCl, sodium citrate, disodium citrate, PSA, C 18 According to the mixture with a mass ratio of 10:5:1:1:2:1; continue to vortex for 3 minutes, centrifuge at 5000r / min, and filter to obtain the supernatant, which is the organic phase extract of ZEN toxin.

[0047] Preparation of Ag sol: The present invention adopts a one-pot method of Ag sol to enhance the Raman detection signal of ZEN azo reaction product. Ag sol was prepared by reducing AgNO with sodium citrate 3 According to the method, Ag nanoparticles with particle size of 80-100nm were synthesized. First take 1m...

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Abstract

The invention discloses a method for rapidly and accurately detecting zearalenone toxin in grains based on SERS (Surface Enhanced Raman Scattering). The method comprises the following steps: (1) carrying out zearalenone toxin azo reaction; (2) collecting a standard SERS spectrogram; (3) fitting a standard curve; according to the method, after the grain sample is simply extracted, the extracted ZEN is subjected to azo reaction with the azo reaction reagent and the auxiliary reagent, the azo product has a very strong SERS signal, the azo product is detected by using a portable Raman spectrometer, and ultra-sensitive detection of the ZEN toxin in the grain product is realized; the method provided by the invention is simple to operate, low in cost and high in speed, does not need a large precise instrument, and can realize outdoor on-site portable detection of grain products; operation of professional technicians is not needed, the requirement for professional knowledge of detection personnel is not needed, ordinary people can rapidly master and carry out detection, and time and cost are greatly saved.

Description

technical field [0001] The invention belongs to the technical field of rapid food detection, and in particular relates to a method for rapidly and accurately detecting zearalenone toxin in grains based on SERS. Background technique [0002] Zearalenone (Zearalenone, ZEN) is mainly produced by Fusarium graminearum, isolated from corn with scab, and is a metabolite of Gibberella zeae. It has estrogen effect and has many adverse reactions to animals. It not only affects the reproductive function of animals, but also produces immunotoxicity, cytotoxicity and genotoxicity, and has certain toxic effects on the nervous system, heart, kidney, liver and lungs, and even Cause abnormal reproductive function of animals leading to death. ZEN pollution has a wide range, deep degree, and great harm, and it exists widely in food raw materials and feedstuffs all over the world. In my country, it mainly pollutes grains such as corn, wheat, rice, barley, millet and oats, which not only poses...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65G01N1/28G01N1/34
CPCG01N21/658G01N1/34G01N1/28
Inventor 李剑锋刘圣红
Owner XIAMEN UNIV
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