CN113952966A - Tungsten diselenide or molybdenum diselenide/gold nanoparticle composite material and preparation method thereof - Google Patents

Tungsten diselenide or molybdenum diselenide/gold nanoparticle composite material and preparation method thereof Download PDF

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CN113952966A
CN113952966A CN202111397417.2A CN202111397417A CN113952966A CN 113952966 A CN113952966 A CN 113952966A CN 202111397417 A CN202111397417 A CN 202111397417A CN 113952966 A CN113952966 A CN 113952966A
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diselenide
tungsten
molybdenum
composite material
gold nanoparticle
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洪诚毅
陈玲玲
黄志勇
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Jimei University
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    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
    • B01J27/057—Selenium or tellurium; Compounds thereof
    • B01J27/0573—Selenium; Compounds thereof
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Abstract

The invention relates to a preparation method of a tungsten diselenide or molybdenum diselenide/gold nanoparticle composite material, which comprises the following steps: stirring the tungsten diselenide nanosheet solution or the molybdenum diselenide nanosheet solution at a constant speed, keeping an ice bath, dropwise adding tetrachloroauric acid into the tungsten diselenide nanosheet solution or the molybdenum diselenide nanosheet solution, reacting for 20min, centrifuging, and collecting precipitates to obtain the tungsten diselenide or molybdenum diselenide/gold nanoparticle composite material. The method is green and simple, has low cost, high efficiency and short production period, and the prepared tungsten diselenide/gold nanoparticle composite material has higher peroxidase catalytic activity and has wide application prospect in the detection of small biological molecular substances such as glucose.

Description

Tungsten diselenide or molybdenum diselenide/gold nanoparticle composite material and preparation method thereof
Technical Field
The invention relates to the field of biomedicine, in particular to a tungsten diselenide or molybdenum diselenide/gold nanoparticle composite material and a preparation method thereof.
Background
Two-dimensional (2D) nanomaterials are of interest because of their unique structure and unique properties, including good mechanical, thermal, electronic properties and high catalytic activity. In particular two-dimensional Transition Metal Dichalcogenides (TMDCs), such as tungsten disulphide (WS)2) Molybdenum disulfide (MoS)2) Tungsten diselenide (WSe)2) And molybdenum diselenide (MoSe)2) Have become promising candidates for biocatalysts, biosensors and biomedical applications.
Glucose is used as a main energy source of living cells, and can rapidly supplement energy, stimulate calcium absorption, strengthen memory and the like. Glucose is closely related to metabolism of human body, and when the glucose content in blood is too high, a series of endocrine and metabolic diseases, such as diabetes, kidney failure and the like, can be caused; but at low concentrations, stroke and damage to brain structures can result. Therefore, rapid and accurate glucose detection is critical to the detection of physiological health and the treatment of diabetes and is of great significance.
Tungsten disulfide (WS) is used in the related art2) Or molybdenum disulfide (MoS)2) The peroxidase mimic enzyme is used for detecting glucose, but has limited catalytic activity.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. Therefore, the invention aims to provide a tungsten diselenide or molybdenum diselenide/gold nanoparticle composite material and a preparation method thereof. The method is green and simple, has low cost, high efficiency and short production period, and the prepared composite material has higher peroxidase catalytic activity and wide application prospect in the detection of small biological molecular substances such as glucose.
Therefore, in one aspect of the invention, the invention provides a preparation method of a tungsten diselenide or molybdenum diselenide/gold nanoparticle composite material, which comprises the following steps:
stirring the tungsten diselenide nanosheet solution or the molybdenum diselenide nanosheet solution at a constant speed, keeping an ice bath, dropwise adding tetrachloroauric acid into the tungsten diselenide nanosheet solution or the molybdenum diselenide nanosheet solution, reacting for 20min, centrifuging, and collecting precipitates to obtain the tungsten diselenide or molybdenum diselenide/gold nanoparticle composite material.
According to the preparation method of the tungsten diselenide or molybdenum diselenide/gold nanoparticles, tungsten diselenide or molybdenum diselenide nano materials are used as a substrate, and the gold nanoparticles are synthesized on the substrate in situIn AuNPs, the single thin tungsten diselenide nano material has weaker peroxidase catalysis, and after the AuNPs are modified on the tungsten diselenide nano material, the composite material has obviously improved catalytic performance compared with the single thin tungsten diselenide nano material. The prepared WSe2Use of AuNPs composite as catalytic H2O2A peroxidase mimic enzyme that oxidizes 3,3',5,5' -Tetramethylbenzidine (TMB) for colorimetric detection of glucose in serum. In addition, the provided method is green and simple, low in cost, high in efficiency and short in production period.
In addition, the preparation method of tungsten diselenide or molybdenum diselenide/gold nanoparticles provided by the above embodiments of the present invention may further have the following additional technical features:
optionally, the concentration of tetrachloroauric acid is 1 mM.
Optionally, the concentration of the tungsten diselenide nanosheet solution or the molybdenum diselenide nanosheet solution is 0.1mg/mL,
optionally, the ratio of the tungsten diselenide nanosheet solution or the molybdenum diselenide nanosheet solution to the tetrachloroauric acid is 10: 1.
alternatively, the centrifugation conditions are 5000rpm, 20 min.
The invention also provides a tungsten diselenide or molybdenum diselenide/gold nanoparticle composite material which is prepared by the method.
The tungsten diselenide/gold nanoparticle composite material has good peroxidase catalytic activity and has wide application prospect in detection of small biological molecular substances such as glucose.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
FIG. 1 is a WSe of the present invention2Nanosheet and WSe2-TEM images of AuNPs composites;
FIG. 2 is a WSe of the present invention2-EDS spectrum of AuNPs composite;
FIG. 3 is a WSe of the present invention2Nanosheet and WSe2-XPS spectra of AuNPs composites;
FIG. 4 is a WSe of the present invention2And WSe2-uv-vis absorption profile of AuNPs catalytic system;
FIG. 5 is a WSe of the present invention2And WSe2-AuNPs catalytic capacity comparison plot;
FIG. 6 shows different pH vs. WSe2-the effect of AuNPs catalytic reactions;
FIG. 7 is a graph of different temperature vs. WSe2-the effect of AuNPs catalytic reactions;
FIG. 8 shows the results of the experiments for detecting hydrogen peroxide and glucose in accordance with the present invention.
Detailed Description
The technical solution of the present invention is illustrated by specific examples below. It is to be understood that one or more method steps mentioned in the present invention do not exclude the presence of other method steps before or after the combination step or that other method steps may be inserted between the explicitly mentioned steps; it should also be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Moreover, unless otherwise indicated, the numbering of the various method steps is merely a convenient tool for identifying the various method steps, and is not intended to limit the order in which the method steps are arranged or the scope of the invention in which the invention may be practiced, and changes or modifications in the relative relationship may be made without substantially changing the technical content.
In order to better understand the above technical solutions, exemplary embodiments of the present invention are described in more detail below. While exemplary embodiments of the invention have been shown, it should be understood that the invention may be embodied in various forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
The test materials adopted by the invention are all common commercial products and can be purchased in the market.
The invention will now be described with reference to specific examples, which are intended to be illustrative only and not to be limiting in any way.
Example 1
Preparation of tungsten diselenide/gold nanoparticle composite material
(1)WSe2-synthesis of AuNPs composite: 3mL of the commercially available WSe was added to a round bottom flask2The nano-sheet solution (0.1mg/mL) is placed on a magnetic stirrer to be stirred at a constant speed and ice bath is kept, and 300 mu L of HAuCl is slowly dripped into a round-bottom flask4After 20min reaction of the solution (1mM), the precipitate was centrifuged and redispersed in water to give WSe2-AuNPs composite material.
Example 2
Preparation of molybdenum diselenide/gold nanoparticle composite material
(1)MoSe2-synthesis of AuNPs composite: 3mL of the obtained MoSe was added to a round bottom flask2The nano-sheet solution (0.1mg/mL) is placed on a magnetic stirrer to be stirred at a constant speed and ice bath is kept, and 300 mu LHAuCl is slowly dripped into a round-bottom flask4After reacting the solution (1mM) for 20min, taking out and centrifuging, and re-dispersing the precipitate in water to obtain MoSe2-AuNPs composite material.
Test examples
And (3) performance testing:
1. and (4) comparing the scanning electron microscope images of the single tungsten diselenide nanosheets.
The results are shown in FIG. 1, and the TEM characterization can verify that AuNPs are successfully modified in WSe2On the nanosheets, the left panel in FIG. 1 is the individual WSe2Nanosheet, right picture is WSe2AuNPs composites in which AuNPs are homogeneously dispersed in WSe2And (4) nano-chips.
2. EDS and XPS characterization:
as shown in FIGS. 2 and 3, the EDS of FIG. 2 shows the presence of gold in the composite, and the energy dispersive x-ray photoelectron spectroscopy (XPS) of FIG. 3 shows loading in WSe2Au on nanosheets, further verifying WSe2Chemical composition of AuNPs composite. As shown in FIG. 3, the XPS spectrum shows W, Se, and Au elements. As shown in FIG. 3(B) (E), the peaks at 54.7 and 55.5eV can be attributed toIs Se 3d orbital binding energy. Meanwhile, as shown in FIG. 3(C) (F), two peaks at 32.5eV and 34.6eV correspond to W4F7/2And W4 f5/2Binding energy. In comparison, Au 4f5/2And Au 4f7/2The characteristic binding energies of (c) are located at 87.9eV and 84.3eV, respectively, in fig. 3 (G). All experimental data confirm WSe2Successful synthesis of AuNPs hybrid structures.
3. Peroxidase catalytic activity
Exploration of WSe by selecting TMB as reaction substrate2-peroxidase mimetic enzyme activity of AuNPs composites. The method comprises adding 25 μ L of nanoenzyme (300 μ g mL) into 96-well plate-1WSe2AuNPs composite materials or WSe2Nanoplatelets). Then 25. mu.L of TMB (10mM), 175. mu.L of LHAc-NaAc (pH 4.0) buffer and 25. mu.L of 5mM H were added2O2The reaction was carried out at 37 ℃ for 30min, and the absorbance was measured at 652 nm.
The results are shown in FIG. 4 and FIG. 5, in FIG. 4, without WSe2Or WSe2In the presence of AuNPs, line a shows H2O2The mixed solution with TMB has almost no absorption at 652 nm; line b is shown at WSe2Under the catalysis of (A) H2O2The mixed solution of TMB and TMB has certain absorption at 652nm, but is not obvious; while in WSe2H is seen from line c in the presence of AuNPs2O2The absorbance of the mixed solution with TMB at 652nm is obviously enhanced, indicating that WSe2AuNPs have very excellent peroxidase activity. As can be seen in FIG. 5, WSe2The catalytic activity of the AuNPs nano material is obviously higher than that of WSe2Nanosheets.
4. For WSe under different temperature and pH conditions2The effect of AuNPs composites on catalytic reactions.
As shown in fig. 6 and 7, it can be seen from fig. 6 that when the pH of the buffer is changed within the range of 2.0 to 9.0 under the other reaction conditions, there is a significant difference in the absorbance value of the measured solution, which first increases, reaches a peak at pH 4.0, and then decreases, as determined from fig. 6. Therefore, the pH of the acetic acid-sodium acetate buffer solution was selected to be 4.0 as the optimum pH for the reaction. In FIG. 7, the absorbance of the solution measured at 625nm increased rapidly with increasing temperature, and reached a maximum at 45 ℃.
5. Detecting hydrogen peroxide and glucose
Hydrogen peroxide (H) under optimized reaction conditions2O2) And glucose. The detection method comprises the following steps: 30 μ L of glucose (10, 20, 50, 100, 200, 500, 1000 and 2000 μ M) at various concentrations, 20 μ L of glucose oxidase (2mg mL)-1) Incubate at 37 ℃ for 30 min. After completion of the reaction, 25. mu.L of TMB (10mM), 150. mu.L of a buffer solution of LHAc-NaAc (200mM, pH 4.0), and 25. mu.L of LWSe were added to the above solution2AuNPs composite (300. mu.g mL)-1). All solutions were mixed well, incubated at 45 ℃ for 30min and absorbance measured at 652 nm.
The results are shown in FIG. 8, above, and in FIGS. 8(a) and (b), when H is2O2As the final concentration increased from 1. mu.M to 1mM, the absorbance at 652nm increased. As can be seen from FIG. 8(b), H2O2There is a good linear relationship between the final concentration of 1 μ M and 100 μ M, with a ═ 0.004C + 0.22. FIGS. 8(c) and (d) are graphs showing the change in absorbance of the reaction solution with the glucose concentration under the optimum conditions. The absorbance value at 652nm increases with increasing glucose concentration in the range 0.01-0.5mM and is well linear in the range 0.01-0.5mM, with the linear equation a ═ 0.29C + 0.22.
In summary, the invention takes tungsten diselenide or molybdenum diselenide nano material as a substrate, gold nano particle AuNPs are synthesized on the substrate in situ, the single thin layer of tungsten diselenide has weaker peroxidase catalysis, and after the AuNPs are modified on the tungsten diselenide nano material, the composite material has obviously improved catalysis compared with the single thin layer of tungsten diselenide nano material. The prepared WSe2Use of AuNPs composite as catalytic H2O2A peroxidase mimic enzyme that oxidizes 3,3',5,5' -Tetramethylbenzidine (TMB) for colorimetric detection of glucose in serum.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above should not be understood to necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples described in this specification can be combined and combined by those skilled in the art.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.

Claims (5)

1. A preparation method of a tungsten diselenide or molybdenum diselenide/gold nanoparticle composite material is characterized by comprising the following steps:
stirring the tungsten diselenide nanosheet solution or the molybdenum diselenide nanosheet solution at a constant speed, keeping an ice bath, dropwise adding tetrachloroauric acid into the tungsten diselenide nanosheet solution or the molybdenum diselenide nanosheet solution, reacting for 20min, centrifuging, and collecting precipitates to obtain the tungsten diselenide or molybdenum diselenide/gold nanoparticle composite material.
2. The method of claim 1, wherein the concentration of the solution of tungsten diselenide nanosheets or molybdenum diselenide nanosheets is 0.1mg/mL and the concentration of tetrachloroauric acid is 1 mM.
3. The method of claim 1, wherein the volume ratio of the solution of tungsten diselenide nanosheets or the solution of molybdenum diselenide nanosheets to tetrachloroauric acid is 10: 1.
4. the method of claim 1, wherein the centrifugation conditions are 5000rpm for 20 min.
5. A tungsten diselenide or molybdenum diselenide/gold nanoparticle composite material, characterized in that the tungsten diselenide or molybdenum diselenide/gold nanoparticle composite material is prepared by the preparation method according to any one of claims 1 to 4.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108445142A (en) * 2018-03-12 2018-08-24 国家纳米科学中心 A kind of application of rhodium piece nano enzyme in simulating biological enzyme
AU2020100704A4 (en) * 2020-05-05 2020-06-11 Chen, Shumeng Miss A method of synthesis of ultrathin palladium nanosheet with peroxidase mimetic activity for the colorimetric detection of H2O2
US20210155514A1 (en) * 2019-11-25 2021-05-27 Northeastern University Robust flow-through platform for organic contaminants removal
CN113281318A (en) * 2021-05-26 2021-08-20 四川中科微纳科技有限公司 Fluorescent-colorimetric dual-signal detection of Fe3+ and GSH by MoSe2@ Fe nano composite material

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CN108445142A (en) * 2018-03-12 2018-08-24 国家纳米科学中心 A kind of application of rhodium piece nano enzyme in simulating biological enzyme
US20210155514A1 (en) * 2019-11-25 2021-05-27 Northeastern University Robust flow-through platform for organic contaminants removal
AU2020100704A4 (en) * 2020-05-05 2020-06-11 Chen, Shumeng Miss A method of synthesis of ultrathin palladium nanosheet with peroxidase mimetic activity for the colorimetric detection of H2O2
CN113281318A (en) * 2021-05-26 2021-08-20 四川中科微纳科技有限公司 Fluorescent-colorimetric dual-signal detection of Fe3+ and GSH by MoSe2@ Fe nano composite material

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Title
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GAOYAN JIANG ET AL.: "Accelerating the peroxidase-like activity of MoSe2 nanosheets at physiological pH by dextran modification", 《CHEM. COMMUN.》, vol. 56, pages 10847 - 10850 *

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