SERS Raman substrate, preparation method thereof and pesticide residue analysis and detection method

A Raman substrate and seed technology, applied in the field of analysis and detection of pesticide residues, can solve problems such as poor mutual solubility and cumbersome chemical synthesis, and achieve the effects of improving sensitivity, reducing detection limit, and improving method sensitivity.

Active Publication Date: 2020-12-01
SHAANXI SCI TECH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, for liquid samples, the premise of the mixing method is that the analyte and the Raman substrate have the same properties, otherwise the miscibility is not good; and for solid samples, simple mixing cannot reduce the interaction between the two very well. distance
In addition, targeted modification involves complex chemical synthesis, and there are cumbersome problems

Method used

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  • SERS Raman substrate, preparation method thereof and pesticide residue analysis and detection method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] (1) 0.278g of ferrous sulfate and 0.54g of ferric chloride were added to a mixture containing 10.0mL of ultrapure water (distilled water was passed through N 2 In deoxygenation 30min), stir at 150r / min for 5min; under 500r / min mechanical stirring, adjust the pH value to 10-11 until the yellow precipitate gradually dissolves into an orange-yellow solution, under the condition of 60 ℃ water bath and stirring, add to the solution Add 1.0 mL of concentrated ammonia water to obtain a black solution, and continue to stir for 30 minutes;

[0039] (2) Ageing the black solution in a water bath at 80°C for 9 to 11 minutes, cooling to room temperature and performing magnetic separation, washing with secondary water until the supernatant is neutral, dispersing the washed product in secondary water, and ultrasonically oscillating for 10 minutes Its solid particles are completely dispersed in water, and the product is centrifuged and separated to obtain magnetic Fe 3 O 4 .

Embodiment 2

[0041] 1 mL of HAuCl with a mass concentration of 1% 4 The solution was added to 90 mL of distilled water, stirred evenly at room temperature, 2.0 mL of sodium citrate solution with a mass concentration of 1% was added, and 1 mL of freshly prepared NaBH with a mass concentration of 0.075% was added after stirring evenly. 4 The solution was stirred for 5 min to obtain a nano-gold seed solution.

Embodiment 3

[0043] (1) 2.1136g Ca(NO 3 ) 2 ·4H 2 O and 3.201g Na 2 HPO 4 were dissolved in 50mL ultrapure water to obtain solutions; 0.20g magnetic Fe 3 O 4 added to Ca(NO 3 ) 2 medium, ultrasonic for 5 minutes, mechanical stirring to form a suspension;

[0044] (2) The suspension was added to the above solution, and the pH value was adjusted to 11±0.5 by 0.1mol / L ammonia water, the stirring reaction was sufficient, the reaction solution was aged at room temperature for 24h, magnetically separated, washed and dried, Magnetic hydroxyapatite is obtained.

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Abstract

The invention discloses an SERS Raman substrate, a preparation method thereof and a pesticide residue analysis and detection method. The preparation method comprises the steps of adding secondary water and an HAuCl4. 4H2O solution into a nanogold seed solution under the atmosphere of mechanical stirring and inert gas to obtain a solution 1, and repeatedly dropwise adding a FeSO4. 7H2O solution and an HAuCl4. 4H2O solution into the solution 1 for four times to obtain a sea urchin-shaped nanogold solution; adding magnetic hydroxyapatite into distilled water, carrying out ultrasonic treatment and magnetic separation, adding polyethyleneimine, carrying out ultrasonic treatment for 0.5 h, taking out a reaction product, adding the reaction product into the sea urchin-shaped nanogold solution, and carrying out ultrasonic treatment to obtain a solution 2; adding a silver-ammonia solution into the solution 2, dropwise adding hydrazine hydrate, reacting for 1 hour, and performing magnetic separation, washing and drying to obtain the SERS Raman substrate Fe3O4 / HAp / Au / Ag. According to the analysis and detection method disclosed by the invention, the SERS Raman substrate material and a Raman sample injection device are combined for application, so that the detection limit of Raman detection can be reduced to a greater extent, the determination of low-concentration substances is realized, and the sensitivity of the method is greatly improved.

Description

technical field [0001] The invention belongs to the field of analysis and detection of pesticide residues, in particular to a SERS Raman substrate, its preparation and a method for analysis and detection of pesticide residues. Background technique [0002] In recent years, with the continuous development of society, pesticide residues have seriously endangered human life and health, and have become a major problem that plagues human beings. Pesticide residues are widely found in agricultural and sideline products, cash crops and other products; on the one hand, pesticide residues endanger human health; on the other hand, they reduce product quality and revenue. The key to improving the quality of agricultural and sideline products is to develop high-sensitivity, high-efficiency, and simple detection technology to achieve accurate analysis and detection of low-level pesticide residues. At the same time, improving the extraction of active ingredients from economic crops such a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65
CPCG01N21/658
Inventor 吴睿
Owner SHAANXI SCI TECH UNIV
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