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A preparation method of electrochemical nonylphenol sensor based on doped titanium dioxide/molybdenum disulfide composite material

A technology of molybdenum disulfide and composite materials, which is applied in the field of preparation of electrochemical biosensors, can solve the problems of cumbersome process and low yield, and achieve the effect of simple preparation, low cost and increased electron transfer capacity

Inactive Publication Date: 2019-03-12
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, most of the synthesis methods are synthesized separately, and then compound the catalyst and the carrier, the process is cumbersome and the yield is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1 Cu-TiO 2 / MoS 2 preparation of

[0038] (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;

[0039] (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;

[0040] (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;

[0041] (4) The reaction product obtained in step (3) was centrifuged and washed three times with ultrapure water and absolute ethanol, and the...

Embodiment 2

[0046] Example 2 Cu-TiO 2 / MoS 2 preparation of

[0047] (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;

[0048] (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;

[0049] (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;

[0050] (4) The reaction product obtained in step (3) was centrifuged and washed three times with ultrapure water and absolute e...

Embodiment 3

[0055] Example 3 Preparation method of electrochemical nonylphenol sensor

[0056] (1) Using ITO conductive glass as the working electrode, drop-coat 8 µL of Cu-TiO on the surface of the electrode 2 / MoS 2 Sol, dry at room temperature;

[0057] (2) Wash the electrode obtained in step (1) with the buffer solution PBS, continue to drop-coat 8 µL of 10 µg / mL nonylphenol antibody solution on the surface of the electrode, and store it in a refrigerator at 4 °C to dry;

[0058] (3) Wash the electrode obtained in step (2) with PBS, continue to drip-coat 8 µL of bovine serum albumin solution with a concentration of 100 µg / mL on the surface of the electrode, and store it in a refrigerator at 4 °C to dry;

[0059] (4) Wash the electrode obtained in step (3) with PBS, store and dry in a refrigerator at 4°C, and then prepare an electrochemical nonylphenol sensor;

[0060] The Cu-TiO 2 / MoS 2 The sol is 50 mg of Cu-TiO 2 / MoS 2 The powder was dissolved in 10 mL ultrapure water, and ...

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Abstract

The invention discloses a preparation method of an electrochemical biosensor. The present invention firstly prepares a new two-dimensional nano-electrode material - doped titanium dioxide / molybdenum disulfide composite material Cu-TiO2 / MoS2, that is, a two-dimensional nanocomposite material in which copper-doped titanium dioxide nano-squares are in-situ compounded with molybdenum disulfide. Taking advantage of the good biocompatibility and large specific surface area of ​​this material, the nonylphenol antibody is loaded, and during detection, because copper-doped titanium dioxide can catalyze hydrogen peroxide to generate O2 in situ, generate electrochemical signals, and reuse The effect of the specific quantitative binding of the antibody to the antigen on the electron transport ability reduces the current intensity accordingly, and finally realizes the construction of a biosensor for the detection of nonylphenol by a label-free electrochemical method.

Description

technical field [0001] The invention relates to a preparation method of an electrochemical biosensor. 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. Nonylphenol is a bisphenol-like synthetic estrogen. At present, the methods for detecting nonylphenol mainly include chromatography and mass spectrometry. Such methods require expensive instruments and complex operations, and laboratory personnel need professional training before they can perform...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/327G01N27/48G01N27/26G01N21/76
CPCG01N21/76G01N27/26G01N27/3275G01N27/48
Inventor 张勇杜斌马洪敏吴丹范大伟
Owner UNIV OF JINAN
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