Preparation method of photoelectrochemical diethylstilbestrol sensor based on copper-doped nano photoelectric material

A technology of diethylstilbestrol and photoelectrochemistry, which is applied in the direction of material electrochemical variables, can solve the problems of low sensitivity of photoelectrochemical sensors, weakening of photoelectric signals, and unfavorable practical applications, so as to broaden the range of photosensitive wavelengths, save time, and increase light. The effect of catalytic activity

Inactive Publication Date: 2016-10-12
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In addition, the photogenerated electron-hole pairs of a single titanium dioxide nanomaterial are easy to recombine, which leads to the weakening of the photoelectric signal, and the poor conductivity of titanium dioxide also limits the sensitivity of photoelectrochemical sensors constructed from a single titanium dioxide nanomaterial. application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Example 1 Cu-TiO 2 / MoS 2 preparation of

[0041] (1) Add 0.6 g of molybdenum disulfide powder and 0.2 mmol of copper salt to 3 mL of n-butyllithium solution, and stir for 12 hours under nitrogen protection at 60 °C to obtain the reacted solution;

[0042] (2) Wash the reacted solution in step (1) with a non-polar solvent, and then perform ultrasonic treatment in a water bath at 60 °C. After the treatment, wash the treated solution with a non-polar solvent, and dry it in vacuum to obtain copper Intercalated molybdenum disulfide nanomaterials;

[0043] (3) Take 500 mg of copper-intercalated molybdenum disulfide nanomaterials prepared in step (2) and add them to 5 mL of tetrabutyl titanate. After stirring for 1 hour, slowly add 0.5 mL of hydrofluoric acid while stirring, and then Reaction in the reactor at 160°C for 18 hours;

[0044] (4) The reaction product obtained in step (3) was centrifuged and washed three times with ultrapure water and absolute ethanol, and...

Embodiment 2

[0049] Example 2 Cu-TiO 2 / MoS 2 preparation of

[0050] (1) Add 0.6 g of molybdenum disulfide powder and 1.0 mmol of copper salt to 5 mL of n-butyllithium solution, and stir for 24 hours under nitrogen protection at 30 °C to obtain the reacted solution;

[0051] (2) Use a non-polar solvent to wash the solution after the reaction in step (1), and then perform ultrasonic treatment in a water bath at 30 °C. After the treatment, use a non-polar solvent to wash the treated solution, and dry it in vacuum to obtain copper Intercalated molybdenum disulfide nanomaterials;

[0052] (3) Take 200 mg of copper-intercalated molybdenum disulfide nanomaterials prepared in step (2) and add them to 5 mL of tetrabutyl titanate. After stirring for 1 hour, slowly add 0.6 mL of hydrofluoric acid while stirring, and then Reaction in the reactor at 180°C for 20 hours;

[0053] (4) The reaction product obtained in step (3) was centrifuged and washed three times with ultrapure water and absolu...

Embodiment 3

[0058] Example 3 Cu-TiO 2 / MoS 2 preparation of

[0059] (1) Add 0.6 g of molybdenum disulfide powder and 2.0 mmol of copper salt to 10 mL of n-butyllithium solution, and stir for 48 hours under nitrogen protection at 50 °C to obtain the reacted solution;

[0060] (2) Wash the reacted solution in step (1) with a non-polar solvent, and then perform ultrasonic treatment in a water bath at 50 °C. After the treatment, wash the treated solution with a non-polar solvent, and dry it in vacuum to obtain copper Intercalated molybdenum disulfide nanomaterials;

[0061] (3) Take 10 mg of copper-intercalated molybdenum disulfide nanomaterials prepared in step (2) and add them to 5 mL of tetrabutyl titanate. After stirring for 1 hour, slowly add 0.8 mL of hydrofluoric acid while stirring, and then Reaction in the reactor at 200°C for 24 hours;

[0062] (4) The reaction product obtained in step (3) was centrifuged and washed three times with ultrapure water and absolute ethanol, and...

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Abstract

The invention discloses a preparation method of a photoelectrochemical diethylstilbestrol sensor and belongs to the technical field of novel nano functional materials and biosensors. Firstly, a novel two-dimensional nano photoelectric material, namely a copper-doped nano photoelectric material, specifically a two-dimensional nano composite Cu-TiO2 / MoS2 obtained through in-situ compounding of molybdenum disulfide on a copper-doped titanium dioxide nano cube is prepared, and an diethylstilbestrol antibody is loaded and alkaline phosphatase is fixed to the material by the application of good biocompatibility and a large specific surface area of the material. During detection, due to the fact that alkaline phosphatase can catalyze L-ascorbic acid-2-trisodium phosphate AAP to generate L-ascorbic acid AA in situ and then provide an electron donor for photoelectric detection, by the application of the influences of specific quantitative combination of the antibody and an antigen on electron transmission capacity, the photoelectric current intensity is lowered accordingly, and finally the photoelectric sensor for detecting diethylstilbestrol through an unmarked photoelectrochemical method is constructed.

Description

technical field [0001] The invention relates to a preparation method of a photoelectrochemical diethylstilbestrol sensor. It belongs to the technical field of new nanometer functional materials and biosensors. Background technique [0002] Environmental estrogen refers to a class of compounds that interfere with the synthesis, release, transport, binding, and metabolism of normal endocrine substances in the body after entering the body, activate or inhibit the function of the endocrine system, and thereby destroy the stability and regulation of the body. There are many kinds of environmental estrogens, including synthetic compounds and plant natural estrogens, which are widely distributed in nature. Diethylstilbestrol is a synthetic non-steroidal estrogen substance. At present, the methods for detecting diethylstilbestrol mainly include chromatography and mass spectrometry. Such methods require expensive instruments and complex operations, and laboratory personnel need pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/26
CPCG01N27/26
Inventor 张勇孙旭魏琴李燕马洪敏
Owner UNIV OF JINAN
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