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A eu for the detection of pesticide residues 3+ Preparation method of labeled molecularly imprinted sensor

A technology for labeling molecules and molecular imprinting, applied in the field of materials science, can solve the problems of small number of recognition sites, poor sensitivity, no signal output, etc., and achieve the effect of high selectivity and high sensitivity trace detection.

Active Publication Date: 2017-12-08
HEFEI UNIV
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Problems solved by technology

[0015] The purpose of the present invention is to solve the shortcomings of the traditional molecular imprinting materials in the current prior art, such as the small number of recognition sites, slow binding kinetics, poor sensitivity and no signal output after binding target analytes. The present invention utilizes Eu 3+ It can coordinate and chelate with the electron-rich amino group in 3-aminopropyltriethoxysilane and the target analyte molecule (pesticide molecule). Under alkaline conditions, 3-aminopropyltriethoxysilane and orthosilicic acid Hydrolysis of ethyl ester yields silica nanoparticles with Eu bound in the particle matrix 3+ Coordination chelation derivatives with amino groups and target analytes, after chelation of target analyte molecules Eu 3+ Fluorescence intensity enhancement, Eu in silica nanoparticle matrix 3+ Coordination and chelation form molecularly imprinted sensors with fluorescent properties. Therefore, the application of rare earth chelation luminescence and molecular imprinting technologies in the detection of pesticide residues can be explored

Method used

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  • A eu for the detection of pesticide residues <sup>3+</sup> Preparation method of labeled molecularly imprinted sensor
  • A eu for the detection of pesticide residues <sup>3+</sup> Preparation method of labeled molecularly imprinted sensor
  • A eu for the detection of pesticide residues <sup>3+</sup> Preparation method of labeled molecularly imprinted sensor

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preparation example Construction

[0054] A kind of Eu for the detection of pesticide residues 3+ Preparation method of labeled molecularly imprinted sensor, including Eu 3+ Pre-assembled with 3-aminopropyltriethoxysilane and the pesticide target analyte, chlorpyrifos, to obtain Eu after hydrolysis and condensation 3+ The labeled chlorpyrifos molecularly imprinted silica nanoparticle sensor is characterized in that: the Eu 3+ After the template molecule chlorpyrifos is eluted from the labeled chlorpyrifos molecularly imprinted silica nanoparticle sensor, it has a selective recognition site for the target analyte chlorpyrifos molecule, and the target analyte chlorpyrifos molecule enters the recognition site of the silica nanoparticle sensor After the point, it will be further compared with the Eu on the recognition site 3+ Chelation occurs, based on the principle of rare earth chelation luminescence, the target analyte chlorpyrifos molecules and Eu 3+ The luminous efficiency after chelation increases, and the...

Embodiment 1

[0058] Example 1: According to the principle of rare earth chelation luminescence, using Eu 3+ Chelate with the amino group in the target molecule, 3-aminopropyltriethoxysilane, and obtain Eu after mutual hydrolysis and cross-linking with ethyl orthosilicate under alkaline conditions 3+ labeled molecularly imprinted SiO 2 Nanoparticle sensor. Specific steps are as follows:

[0059] Weigh 0.0312g of Eu 2 o 3 Put it in a 25mL beaker, add 250μL of concentrated nitric acid and 1300uL of deionized water to it, and sonicate for 7 min, until the solution is clear, to obtain Eu(NO 3 ) 3 solution. Take 0.0368g of chlorpyrifos and ultrasonically dissolve it in the ethanol solution, then add 240 μL of 3-aminopropyltriethoxysilane to the solution, then add this solution to the previously prepared Eu(NO 3 ) 3 Solution, then put the solution in a 250mL round bottom flask, ultrasonic 9min, after standing still for 28min, add 2.9mL tetraethyl orthosilicate, adjust the pH to 10 with am...

Embodiment 2

[0060] Embodiment 2: Eu by weighing 0.0180g 2 o 3 Place in a 25mL beaker, add 240μL of concentrated nitric acid and 1300uL of deionized water to it, and ultrasonicate for 6 minutes. After the solution is clarified, Eu(NO 3 ) 3 solution. Get 0.0240g of imidacloprid ultrasonically dissolved in ethanol solution, then add 220 μL of 3-aminopropyltriethoxysilane to the solution, then add this solution to the previously prepared Eu(NO 3 ) 3 Solution, then put the solution in a 250mL round bottom flask, ultrasonic 9min, after standing still for 30min, add 2.5mL tetraethyl orthosilicate, adjust the pH to 10 with ammonia water, add 85mL ethanol water, so that the volume of the solution is adjusted to 100mL , put the solution on a magnetic stirrer, stir at 750rpm for 5min, then gently stir (at a fixed speed of 500rpm) for 5h. . Take 90mL of concentrated nitric acid, put it into a 500mL volumetric flask, and prepare 1moL·L -1 HNO 3 , add HNO to three centrifuge tubes 3 , centrif...

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Abstract

The invention relates to a method for preparing a Eu3+ labelled molecule imprinted sensor used for pesticide residue detection and belongs to the technical field of environment functional material preparation. The method comprises the steps that Eu3+ and amino groups and pesticide residue molecules in APTS are pre-organized and then subjected to hydrolytic crosslinking condensation with TEOS so that the Eu3+ labelled pesticide residue molecule imprinted silicon dioxide nanoparticle sensor can be obtained, pesticide residue molecule selective recognition site holes are obtained after pesticide residue molecules are eluted, chelation between pesticide residue molecules and Eu3+ on a recognition site is conducted after the pesticide residue molecules enter the recognition site of the sensor again, the fluorescence intensity of the pesticide residue molecules is improved after being chelated with Eu3+, and then high-selectivity, high-binding-capacity and high-sensitivity detection of the trace pesticide residue molecules is achieved by means of the change of the fluorescence intensity. The obtained Eu3+ labelled molecule imprinted sensor has the advantages that the rigidity of the recognition site is high, Eu3+ is not prone to elution, repeated utilization can be achieved, solvent inertness, light stability and single dispersity are high, and size is uniform.

Description

technical field [0001] The invention relates to the field of material science, in particular to Eu 3+ Preparation method of labeled molecularly imprinted sensor. Background technique [0002] From the perspective of social development, the emergence and development of pesticides has greatly promoted the progress of human society. However, from the perspective of environmental protection and food safety, pesticides have the characteristics of high residue and high stability, which can cause serious harm to human health. Therefore, in recent years, the detection of trace pesticides and the exploration of related sensors It has attracted extensive attention and fruitful explorations from social research institutions. The laboratory detection of trace pesticide residues (referred to as pesticide residues) has been widely used through gas chromatography atomic emission, gas chromatography-mass spectrometry (GC-MS method) and immunoassay techniques. These traditional analytical...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/64
Inventor 高大明江晓敏郑传阳许梦菡侯婷婷周杨群陈红朱德春
Owner HEFEI UNIV
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