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Preparation method of modified magnetic composite nano particles and application thereof in pesticide detection

A magnetic composite nanometer and composite nanoparticle technology, applied in the fields of food safety testing and nanomaterial technology, can solve the problems such as the inability of the nanocomposite substrate to meet the detection limit requirements, and achieve the improvement of SERS detection sensitivity and specificity, consistent particle morphology, The effect of shortening the detection time

Active Publication Date: 2019-09-17
深圳市农产品质量安全检验检测中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the detection of more trace organic pollutants or pesticide residues is required, Ag / Fe 3 o 4 Nanocomposite substrates fail to meet detection limit requirements
In addition, there is currently no application of magnetic nanoparticles in the detection of thiabendazole

Method used

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  • Preparation method of modified magnetic composite nano particles and application thereof in pesticide detection
  • Preparation method of modified magnetic composite nano particles and application thereof in pesticide detection
  • Preparation method of modified magnetic composite nano particles and application thereof in pesticide detection

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Example 1 Magnetic Fe 3 o 4 Preparation of NPs

[0039] Synthesized by solvothermal synthesis, 8.1 g of FeCl 3 ·6H 2 O was added to 70ml of ethylene glycol, mixed and stirred at 60°C for 10min, and then 7.2g of NaAc·3H was added to the above solution 2 O and 2.0 g of sodium citrate, stirred vigorously at 60°C for 30min, transferred to a polytetrafluoroethylene-lined stainless steel reaction kettle, sealed and placed in an electric blast drying oven at 200°C for 10h; after natural cooling, magnetic collection , washed three times with ethanol, and the precipitate was dried for later use; see figure 2 (a), These rough-surfaced spherical Fe3O4 nanoparticles have uniformly distributed sizes with an average diameter of about 300 nm.

Embodiment 2

[0040] Example 2 Fe 3 o 4 @SiO 2 Preparation of NPs

[0041] Fe 3 o 4 Nanoparticles (0.1g) were added containing 10ml water, 180ml ethanol and 8ml NH 3 ·H 2 O mixture solution, after 30 minutes of ultrasonic treatment, so that it is well dispersed in the solution. Then, slowly add 0.8ml TEOS to the above solution and stir; after reacting for 2 hours, collect again by magnetic force and wash with ethanol and deionized water. Finally, dry at 60°C for later use; see figure 2 (b), the average diameter increased to 330nm, and the spherical structure remained unchanged, proving that SiO 2 shell in Fe 3 o 4 The coating on NPs is uniform. with Fe 3 o 4 NPs compared to SiO 2 The surface is smooth and the transparency is higher, which is also SiO 2 Features of the enclosure. Therefore, the core-shell structure can be observed, and the changes in their surface morphology and particle size are obvious, indicating that the synthesis of different products at each step is s...

Embodiment 3

[0042] Example 3 Fe 3 o4 @SiO 2 Preparation of @Ag NPs

[0043] 0.1g of Fe 3 o 4 @SiO 2 Nanoparticles were dispersed in 15ml of ethanol by ultrasonication for 5min, and then 5ml of HCl with a volume concentration of 5% and 10ml of SnCl with a concentration of 10g / L were added to the above solution 2 , 20min sonication. Then, the obtained composite nanoparticles were separated from the solution by magnetic force, and then quickly rinsed three times with deionized water; then 10 ml of PVP aqueous solution with a concentration of 2 g / L was added to fresh [Ag(NH 3 ) 2 ] + solution, where fresh [Ag(NH 3 ) 2 ] + The solution consists of 5ml of AgNO with a concentration of 12g / L 3 The solution was added with 25ml of NH 3 ·H 2 O is prepared; the composite nanoparticles obtained by step (2) are redispersed in the above-mentioned mixed solution; adding 12ml concentration is 12g / L glucose and 3ml concentration is the sodium tartrate reducing solution of 5g / L, stirring at roo...

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Abstract

The invention discloses a preparation method of modified magnetic composite nano particles and application thereof in pesticide detection. Magnetic composite Fe3O4@SiO2@Ag@COOH NPs are combined with an Au film to form an SERS substrate for effectively detecting trace thiaform bacteria. The Fe3O4@SiO2@Ag@COOH NPs have the same shape, good dispersibility and a core-shell structure, and can be quickly separated from the external magnetic field, so that thiabendazole is enriched. In addition, since LSPR of the Au film is coupled to the SPPs of the Ag particles, the SERS is further enhanced, the sensitivity of the detection is improved, and the rapid detection down to a concentration of 1[mu]g / L is realized.

Description

technical field [0001] The invention belongs to the fields of nanomaterial technology and food safety detection, and in particular relates to a preparation method of modified magnetic composite nanoparticles and its application in pesticide detection. Background technique [0002] Thiabendazole is a commonly used antiseptic and preservative at present. It is often used on fruits and vegetables before or after harvesting. The fruits and vegetables after spraying or dipping can not only prolong the storage time, but also keep freshness and color. These food additives have certain biological toxicity effects, and excessive residues will inevitably have an impact on human health, including thiabendazole. [0003] At present, the detection methods of fruit and vegetable residual preservatives reported at home and abroad mainly involve spectrophotometry, ELISA, high-phase liquid chromatography (HPLC), liquid chromatography-tandem mass spectrometry (LC-MS), gas chromatography-tande...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65B22F1/02B82Y30/00B82Y40/00C01G49/08C01B33/18
CPCG01N21/658B82Y30/00B82Y40/00C01G49/08C01B33/18C01P2004/80B22F1/17B22F1/054
Inventor 但琨胡祥娜禹绍周王瑞林慧纯
Owner 深圳市农产品质量安全检验检测中心
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