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Organophosphorus pesticide molecular probe, preparation and application method thereof and inorganic/organic composite rare earth upconversion nano material

A rare earth upconversion, organophosphorus pesticide technology, applied in the field of pesticide detection, can solve problems such as limited wide application, photobleaching stability of molecular probes, etc.

Active Publication Date: 2016-06-08
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, traditional molecular probes based on fluorescence changes of organic molecules are usually affected by photobleaching and have poor stability, which severely limits their wide application.

Method used

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  • Organophosphorus pesticide molecular probe, preparation and application method thereof and inorganic/organic composite rare earth upconversion nano material
  • Organophosphorus pesticide molecular probe, preparation and application method thereof and inorganic/organic composite rare earth upconversion nano material
  • Organophosphorus pesticide molecular probe, preparation and application method thereof and inorganic/organic composite rare earth upconversion nano material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] NaYF with blue fluorescence 4 :20%Yb,0.1%TmNaYF 4 The preparation of core-shell structure rare earth up-conversion nanoparticles is as follows:

[0064]Accurately weigh yttrium chloride (156.0mg, 0.8mmol), ytterbium chloride (56.0mg, 0.2mmol), and thulium chloride (0.3mg, 0.001mmol) into a 100mL three-necked bottle, then add 7mL oleic acid, 15mL1 -Octadecene, vacuumize at room temperature for 10min; gradually raise the temperature to 160°C, stir for 40min; cool the system to room temperature, transfer it to a 48°C water bath, and then add pre-prepared ammonium fluoride (148mg, 4mmol, 5mL methanol) , sodium hydroxide (100mg, 2.5mmol, 5mL methanol) mixed solution, stirred in a water bath for 40min; then moved the system into a heating mantle, raised the temperature to 75°C, pumped air to remove methanol, then gradually raised the temperature to 300°C, and kept stirring for 1.5h After the end, the system was naturally cooled to room temperature, moved into a 50mL centrif...

Embodiment 2

[0068] The preparation of the core-shell structure nanomaterial modified by Tween 20, its method is as follows:

[0069] Take 20 mg of oleic acid-modified core-shell structure rare earth nanomaterials in a round bottom flask, add 10 mL of cyclohexane, and ultrasonically disperse; add 100 μL of Tween 20, ultrasonically for 15 min, and stir at room temperature for 1 h; slowly drop into 25 mL of ultrapure In water, stir and volatilize cyclohexane at 70°C until the solution is clear; cool at room temperature, centrifuge, and wash with ultrapure water for 3 times, and the solid obtained by centrifugation is dispersed in ultrapure water to obtain the surface Tween 20-modified rare earth upconversion nano particles. Its TEM characterization as figure 2 As shown in b, after water-soluble modification with Tween 20, the particle size and morphology of nanomaterials did not change significantly.

Embodiment 3

[0071] The preparation of inorganic / organic composite rare earth up-conversion nanomaterials, the specific synthesis steps are as follows:

[0072] Weigh 20 mg of Tween 20-modified core-shell structure rare earth nanomaterials, disperse them in 5 mL of N,N-dimethylformamide, then weigh 30 mg of molecular probes and add them, sonicate for 10 min, and then disperse them at room temperature. Stir overnight. Afterwards, the precipitate was collected by centrifugation, washed twice with water, and then the solid was dried to obtain a rare earth nanomaterial loaded with molecular probes. The characterization of its spectroscopic properties is as follows image 3 As shown, the rare earth nanomaterials have strong emission at 475nm and 803nm, and the molecular probe has strong absorption at 475nm, but after reacting with diethyl chlorophosphate, the ultraviolet absorption of the molecular probe at 475nm is sharp reduce.

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Abstract

The invention discloses an organophosphorus pesticide molecular probe, a preparation and application method thereof and inorganic / organic composite rare earth upconversion nano material. The organophosphorus pesticide molecular probe is loaded to the surface of the rare earth upconversion nano material modified by tween to efficiently detect the organophosphorus pesticide concentration in a to-be-detected sample. The organophosphorus pesticide molecular probe has the advantages that the probe is high in sensitivity, good in stability, affordable, capable of achieving ratio type fluorescent detection of organophosphorus pesticide, and capable of providing early sensitive prewarning on the existing possibility of organophosphorus type nerve poison.

Description

technical field [0001] The invention relates to an organophosphorus pesticide molecular probe, a preparation method, an application method thereof and an inorganic / organic composite rare earth up-conversion nano material, belonging to the technical field of pesticide detection. Background technique [0002] In recent years, in order to effectively control pests and obtain higher yields, the use of pesticides has become more and more widespread in agriculture and fruit and vegetable cultivation. But what must be paid attention to is that with the extensive use of pesticides, our environment and health security have also been seriously threatened. According to statistics, the annual use of organophosphorus pesticides in the world is close to one billion pounds, and these pesticides can be detected in soil, food, water resources and even the atmosphere . Int. J. Electrochem. Sci., 2015, 10, 859-869.]. A variety of organophosphorus pesticides have relatively strong toxicity, m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D221/14C09K11/02C09K11/06C09K11/85G01N21/64G01N21/33
CPCC07D221/14C09K11/02C09K11/06C09K11/7773C09K2211/1029G01N21/33G01N21/6428
Inventor 曾文彬王帅亮王晓博
Owner CENT SOUTH UNIV
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