CN111272846A - AuNPs-ZnO-rGO nano composite material synthesized by ultraviolet illumination reduction method and application thereof - Google Patents

AuNPs-ZnO-rGO nano composite material synthesized by ultraviolet illumination reduction method and application thereof Download PDF

Info

Publication number
CN111272846A
CN111272846A CN202010153720.7A CN202010153720A CN111272846A CN 111272846 A CN111272846 A CN 111272846A CN 202010153720 A CN202010153720 A CN 202010153720A CN 111272846 A CN111272846 A CN 111272846A
Authority
CN
China
Prior art keywords
zno
gingerol
aunps
rgo
composite material
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202010153720.7A
Other languages
Chinese (zh)
Inventor
孔粉英
张琳
王玉琴
王伟
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yancheng Institute of Technology
Original Assignee
Yancheng Institute of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Yancheng Institute of Technology filed Critical Yancheng Institute of Technology
Priority to CN202010153720.7A priority Critical patent/CN111272846A/en
Publication of CN111272846A publication Critical patent/CN111272846A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28Electrolytic cell components
    • G01N27/30Electrodes, e.g. test electrodes; Half-cells
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/416Systems
    • G01N27/48Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage

Abstract

The invention discloses an AuNPs-ZnO-rGO nano composite material synthesized by an ultraviolet light reduction method and application thereof. The method comprises the following steps: weighing 5-10mg of graphene oxide, dispersing in 20ml of ultrapure water, and performing ultrasonic treatment for 0.5-1h to obtain a GO dispersion solution; weighing 10-15mg ZnO, dissolving in GO dispersion solution, performing ultrasonic treatment for 0.5-1h, and adding 0.2-0.5mL0.0245M HAuCl4Subjecting the solution to ultrasonic treatment, and then placing the solution in ultraviolet irradiation for 20-30 minutes to obtain a mixture A; and centrifuging the mixture A, and washing and precipitating by using ultrapure water to obtain the nano composite material. The AuNPs-ZnO-rGO nano composite material has good electrocatalysis effect on 6-gingerol, high sensitivity, good stability, selectivity and reproducibility and good application prospect.

Description

AuNPs-ZnO-rGO nano composite material synthesized by ultraviolet illumination reduction method and application thereof
Technical Field
The invention relates to the technical field of nano composite material preparation, in particular to an AuNPs-ZnO-rGO nano composite material synthesized by an ultraviolet light reduction method and application thereof.
Background
The starting point for any high quality sensor development is closely related to the fabrication of the active material and the device design. Inorganic metal oxide nanostructures are a new class of materials for functional device development that exhibit excellent key characteristics, such as stable chemical, thermal, and mechanical properties on the nanometer scale. In fact, recently reported metal oxide based sensors have gained vigorous development in the existing literature due to their key features, in particular their enhanced electrochemical signaling. Among various metal oxide nanomaterials, ZnO nanomaterials are particularly spotlighted because of their unique nano-morphology, non-toxicity, catalytic properties, functional compatibility and other excellent properties. ZnO nanomaterials of various shapes have been produced using different production techniques such as nanofibres through electrostatic spinning, rough nanotopography through radio frequency sputtering, three-dimensional ordered structures through printing techniques, highly controlled structures through electron beam lithography and molecular beam epitaxy and various nanostructured chemical techniques through wet processes. These nanostructures have excellent properties and can be used to fabricate potentially ideal sensing devices with key characteristics such as low detection limits, without any filters, ultra-fast sensing capabilities and recovery, strong reproducibility, good sensitivity, high selectivity and capability to operate at ambient room temperature.
6-Gingerol (6-Gingerol) is a major phenolic compound isolated from plants of the Zingiberaceae family, has been known as a traditional medicine for thousands of years, and has been demonstrated in previous studies to have antitumor activity as a spice flavoring to enhance culinary flavor. The role of 6-gingerol in ameliorating disease has been the focus of research over the last two decades by many researchers who have provided strong scientific evidence of beneficial health. The use of 6-gingerol as a medicinal food derivative appears to be safe in the treatment or prevention of chronic diseases, which would be beneficial to the general population, clinicians, patients, researchers, students and industrialists. Therefore, the detection of 6-gingerol is important and has certain medicinal value.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an AuNPs-ZnO-rGO nano composite material synthesized by an ultraviolet light reduction method and application thereof, wherein the nano composite material has good stability and can be used for high-sensitivity determination of 6-Gingerol. The actual sample is verified, and the developed sensor has the advantages of compactness and high stability.
An AuNPs-ZnO-rGO nano composite material synthesized by an ultraviolet light reduction method comprises the following steps:
step 1, weighing 5-10mg of Graphene Oxide (GO), dispersing in 20ml of ultrapure water, and performing ultrasonic treatment for 0.5-1h to obtain a GO dispersion solution;
step 2, weighing 10-15mg of ZnO, dissolving in GO dispersion solution, carrying out ultrasonic treatment for 0.5-1h, and then adding 0.2-0.5mL0.0245M HAuCl4Carrying out ultrasonic treatment on the solution for 0.5-1h, and then irradiating the solution under an ultraviolet lamp for 20-30 minutes to obtain a mixture A;
step 3, centrifuging the mixture A, and washing and precipitating with ultrapure water to obtain a nano composite material; the resulting nanocomposite was dispersed in ultrapure water and stored at 4 ℃ for use.
The AuNPs-ZnO-rGO nano composite material is applied to the preparation of an electrochemical sensor for detecting 6-gingerol.
In a modification, the electrolyte for detecting 6-gingerol is BR solution.
As an improvement, the pH value of the 6-gingerol is 2.
As an improvement, the sweeping speed of the 6-gingerol detection is 100 mV.
As an improvement, the enrichment time for detecting 6-gingerol is 120 s.
Has the advantages that:
compared with the prior art, the AuNPs-ZnO-rGO nano composite material synthesized by the ultraviolet light reduction method and the application thereof are disclosed, the AuNPs-ZnO-rGO nano composite material is synthesized by the ultraviolet light reduction method, the obtained AuNPs-ZnO-rGO nano composite material has good electrocatalysis effect on 6-Gingerol, and the stability, the selectivity and the reproducibility are good, and the linear range of the 6-Gingerol concentration detection is as follows: 0.1-100 mu M and LOD of 0.03 mu M (S/N is 3), and can be used for high-sensitivity and rapid determination of 6-Gingerol in ginger samples.
Drawings
FIG. 1 is a diagram of ultraviolet absorption spectra, wherein (a) is GO and (b) is AuNPs-ZnO-rGO;
FIG. 2 is a TEM image in which (A) is GO, (B) is ZnO, and (C) is AuNPs-ZnO-rGO;
FIG. 3 is an XPS spectrum of AuNPs-ZnO-rGO nanocomposite, (A) is a complete XPS spectrum, (B) is a high resolution AuNPs 3D XPS spectrum of AuNPs-ZnO-rGO, (C) is the binding energy of Zn 2p3/2 and Zn 2p1/2, (D) is a high resolution C1s spectrum of GO, and (E) is a high resolution C1s spectrum of AuNPs-ZnO-rGO nanocomposite;
FIG. 4 is a graph of CV of AuNPs-ZnO-rGO/GCE in pH2.0BR buffer solution without (a) and with (b) 100. mu.M 6-Gingerol;
FIG. 5 is a CV diagram of naked GCE (a), rGO/GCE (b), ZnO/GCE (c), rGO-ZnO/GCE (d), and rGO-ZnO-Au/GCE (e) in 100. mu.M 6-Gingerol in BR buffer solution at pH 2.0;
FIG. 6 is a graph of Ipa versus pH for 6-Gingerol;
FIG. 7 is a cyclic voltammogram of AuNPs-ZnO-rGO/GCE at different sweep rates in 10. mu.M 6-Gingerol pH2.0 BR;
FIG. 8 is a graph of the square root of Ipa versus sweep rate for 6-Gingerol;
FIG. 9 is a graph of Ipa versus t for 6-Gingerol;
FIG. 10 is a plot of Ipa versus AuNPs-ZnO-rGO nanocomposite dispersion dosage for 6-Gingerol;
FIG. 11 is a graph of LSV responses in AuNPs-ZnO-rGO/GCE at various concentrations of (a-j, 0.1-100. mu.M) 6-Gingerol in buffer solution at pH2.0BR, (A) is a response plot, and (B) is the corresponding linear calibration curve;
FIG. 12 shows the effect of interferents on the assay of 6-Gingerol;
FIG. 13 is a reproduction of a modified electrode;
FIG. 14 is a graph of normalized recovery LSV.
Detailed Description
The invention is further described with reference to specific examples.
In the experiment, the reagents are AR grade and can be purchased from conventional sources, wherein the graphene oxide is prepared for the laboratory.
Example 1 preparation of AuNPs-ZnO-rGO nanocomposites
Weighing 10mg of GO, dispersing in 20ml of ultrapure water, and carrying out ultrasonic treatment for 0.5h to obtain a GO dispersion solution;
weighing 10mg ZnO, dissolving in GO dispersion solution, mixing and ultrasonic treating for 0.5h, and adding 0.2mL 0.0245MHAuCl4Subjecting the solution to ultrasonic treatment for half an hour, and irradiating under ultraviolet lamp for 20min to obtain mixture A.
And centrifuging the mixture A, and washing and precipitating by using ultrapure water to obtain the nano composite material. The resulting nanocomposite was dispersed in ultrapure water and stored at 4 ℃ for use.
Example 2 preparation of AuNPs-ZnO-rGO modified electrode
After polishing a Glassy Carbon Electrode (GCE) with aluminum powder with the particle size of 0.3 μm and 0.05 μm respectively, the surface of the electrode was cleaned with ultrapure water and then washed with ethanol. 6. mu.L, 1 mg/mL of the solution was added dropwise to the GCE surface-1The dispersion liquid of the AuNPs-ZnO-rGO nano composite material is dried in the air for about 8 hours, and the electrode is marked as AuNPs-ZnO-rGO/GCE and is stored at 4 ℃.
The same method is adopted to prepare the electrode used as a comparison electrode, such as a bare electrode, an rGO/GCE electrode, a ZnO/GCE electrode and an rGO-ZnO/GCE electrode. And AuNPs-ZnO-rGO/GCE, ZnO/GCE and rGO-ZnO/GCE are used for carrying out electrochemical detection on 6-Gingerol, and the result is shown in figure 5.
The electrochemical detection comprises the following steps:
a series of 6-gingerols at different concentrations were added to an electrochemical electrolyte containing 10mL of BR buffer. The methods used in the electrochemical performance test in the experiment include CV and LSV, and the test conditions are as follows: the voltage is selected to be 0.00-1.00V, and the sweep rate is 100mV s-1The enrichment step was carried out for an enrichment time of 120 s. The procedure was carried out in CHI 660D, measuring the 6-Gingerol concentration at 1X 10-4M, electrochemical reaction under a BR buffer solution at pH 2.0. Quantitative analysis of 6-Gingerol was performed using peak current at 0.71V (Ipa). The experiment was carried out at room temperature.
Crushed ginger which can be used on ginger is extracted from ginger. Taking 1.0 g of an actual sample (unless otherwise stated), taking 5mL of ethanol as a solvent, violently shaking the actual sample for 1min by using a stirrer, putting the mixed sample into an ultrasonic cleaner for 30min, removing solids from the mixed solution at the rotating speed of 4000r/min for 10min, taking supernatant, collecting and storing the supernatant at 4 ℃ to serve as an experimental sample for later use.
And (3) carrying out performance detection on the nanocomposite.
1. Characterization of
Ultraviolet absorption visible light (UV-Vis) analysis
As shown in FIG. 1, GO shows a strong absorption peak and a broad peak at 235nm and 300nm, respectively, while rGO shows a strong absorption peak at 260 nm. After AuNPs-ZnO-rGO is successfully synthesized, the absorption peak at 235nm of graphene oxide is red-shifted to 258nm, which is consistent with the absorption peak at 260nm in graphene, and thus the graphene oxide is successfully reduced; meanwhile, a strong absorption peak appears at 520nm, which is matched with the absorption peak of AuNPs, thereby proving the successful synthesis of the AuNPs-ZnO-rGO nano material.
2. Transmission electron microscopy analysis
FIG. 2 shows TEM images of GO, ZnO and AuNPs-ZnO-rGO nanocomposites, respectively. As can be seen from fig. 2(a), GO exhibits a typical plate-like shape with slight wrinkles on the surface. It can be seen from fig. 2(B) that the average diameter of the zinc oxide nanoparticles is 10nm, and nano-agglomeration is caused by the high surface energy of the nanocrystals, in accordance with the data table of the supplier. As can be clearly observed from the TEM image of fig. 2(C), a large amount of black AuNPs having an average particle size of about 5nm were well dispersed and attached to the sidewalls and surfaces of ZnO and rGO. AuNPs have no obvious agglomeration phenomenon, and the AuNPs have good dispersibility. Therefore, the ZnO-GO matrix can be used as an auxiliary material of AuNPs with good dispersibility.
3. X-ray photoelectron spectroscopy (XPS) analysis
FIG. 3 shows the XPS spectrum of AuNPs-ZnO-rGO nanocomposites, with the complete XPS spectrum (as in FIG. 3(A)) indicating the presence of elements C, O, Zn and Au. High resolution Au 3d XPS spectra for AuNPs-ZnO-rGO, corresponding to Au 4f7And Au 4f5Has a binding energy of about 84.07 andtwo distinct peaks were present at 87.75 (FIG. 3(B)), indicating successful synthesis of AuNPs. In FIG. 3(C), two sites at 1022.16eV and 1045.16eV represent Zn 2p, respectively3/2And Zn 2p1/2And the energy difference of the binding energy is 23.0 eV. In addition, comparing the peaks of GO and AuNPs-ZnO-rGO nanocomposites of fig. 3(D) and 3(E) with the peak of C1s, it can be seen that the peak intensities of C-O, C ═ O and O-C ═ O are severely reduced, but C-C is increased, indicating efficient GO reduction during uv illumination.
4. Electrochemical behavior research of gingerol on modified electrode
As shown in FIG. 4, curve a is a graph of CV in pH2.0BR in the absence of 6-Gingerol (blank experiment) for AuNPs-ZnO-rGO/GCE; curve b is a CV diagram of AuNPs-ZnO-rGO/GCE in pH2.0BR under the condition of 100 mu M of 6-Gingerol, and the obvious electrocatalytic oxidation effect of AuNPs-ZnO-rGO/GCE on 6-Gingerol can be seen from the CV diagram;
in FIG. 5, curve a is a CV plot of 6-Gingerol in bare GCE showing an irreversible oxidation peak at 0.747V, and Ipa is 2.868 × 10-6A; curve b is a CV diagram of 6-Gingerol on ZnO/GCE, which has an irreversible oxidation peak at 0.729V, and the peak value is 2.946X 10-6A; curve c is a CV diagram of 6-Gingerol at rGO/GCE with an irreversible oxidation peak at 0.711V and an Ipa of 6.118X 10-6A; curve d is a CV diagram of 6-Gingerol on rGO-ZnO/GCE with an irreversible oxidation peak at 0.724V, which is 7.396X 10-6A; curve e is a CV diagram of 6-Gingerol on AuNPs-ZnO-rGO/GCE, which has an irreversible oxidation peak at 0.667V, and the peak value is 1.171X 10-5A. Experimental results show that 6-Gingerol has better current response on AuNPs-ZnO-rGO/GCE. The electrocatalytic oxidation reaction of 6-Gingerol is a completely irreversible electrode reaction process, and the Ipa of 6-Gingerol in AuNPs-ZnO-rGO/GCE is 4 times that of naked GCE, 4 times that of ZnO/GCE, 2 times that of rGO/GCE and 1.6 times that of rGO-ZnO/GCE, which shows that the AuNPs-ZnO-rGO nano composite material has better electrocatalytic oxidation effect on 6-Gingerol.
In this experiment, an electrode with 6. mu.L of AuNPs-ZnO-rGO composite material dropped on the surface and one electrode are usedAnd a bare electrode. Selecting the concentration of 1 × 10-4M6-Gingerol, selecting BR buffer solution with pH of 2.0, selecting voltage range of 0.00-1.00V, and scanning speed of 100mV s-1The test was performed by CV method.
5. Optimization of electrochemical assay methods
(1) Selection of supporting electrolyte
A concentration of 100. mu.M of 6-Gingerol at 0.10M of HCl, H2SO4,H3PO4,HNO3, Tris,Tris-HCl,Tris-HCl-NaCl-MgCl2Ipa in the buffer solution showed that 6-Gingerol had an oxidation peak in the above buffer solution, but the peak current and the peak appearance position were different. 6L of AuNPs-ZnO-rGO composite material is dripped on the polished GCE surface and dried for 6 hours. The concentration of 6-Gingerol is 100 mu M, and 100mV s is used in the potential range of 0.00-1.00V-1The CV test was performed. The addition of the supporting electrolyte can enhance the conductivity of the solution and maintain the strength of stable ions, i.e. the supporting electrolyte can improve the sensitivity and accuracy of the measurement.
This example tests different supporting electrolyte solutions (HCl, H)2SO4,H3PO4,HNO3,Tris,Tris-HCl,Tris-HCl-NaCl-MgCl2Buffer solution) was enhanced over the electrochemical behavior of 6-Gingerol solution on AuNPs-ZnO-rGO/GCE. The results show that 6-Gingerol at a concentration of 100. mu.M has the best electrochemical behavior in BR solution, so BR solution was chosen as supporting electrolyte.
(2) Influence of the pH value
The influence of the pH of the supporting electrolyte on the voltammetric behavior of 6-Gingerol was examined using CV. Different pH values affect the oxidation current peak and the peak position of 6-Gingerol. The results are shown in FIG. 6, from which we can see that the pH is in the range of 1.0-7.0 in paI of 6-GingerolpaIs first increased and then decreased. When the pH is 2.0, the Ipa reaches the maximum value of 2.25X 10-6A. Therefore, in the subsequent experiments, the pH of the BR buffer was chosen to be 2.0. In the experiment, 6L AuNPs-ZnO-rGO is used for modifying GCE. Adding into the mixture at a concentration of 100 μ MThe 6-Gingerol is tested, the voltage range is selected to be 0.00-1.00V, BR is selected, the pH is 1.0-10.0, and the sweep speed is 100mV s-1Then, CV measurement was performed.
6. Current response of AuNPs-ZnO-rGO/GCE at different scanning speeds
The effect of scan speed on the voltammetric behavior of 6-Gingerol on AuNPs-ZnO-rGO/GCE was examined. 6 mu L of AuNPs-ZnO-rGO is dripped on the surface of GCE and dried. In the case of adding 100. mu.M 6-Gingerol, scanning was performed in BR buffer solution at pH2.0, with a voltage selected in the range of 0.00 to 1.00V and a scanning speed selected in the range of 5, 10, 20, 30, 50, 80, 100, 150, 200, 250, 300, 350, 400, 450, 500mV/s (curves a to o in FIG. 7), and the test was performed using CV.
CV diagram of 6-Gingerol on AuNPs-ZnO-rGO/GCE obtained from experimental results, see FIG. 7. It can be seen that the position of Ipa is shifted positively with increasing sweep rate, indicating that the electrochemical reaction of 6-Gingerol on AuNPs-ZnO-rGO nanocomposites is a completely irreversible electrode reaction process.
Then, by comparing the relation between Ipa and square root of scan rate of 6-Gingerol on AuNPs-ZnO-rGO/GCE as shown in FIG. 8, it can be seen from FIG. 8 that scan rate is 10-500mV s-1In between, the oxidation peak current increases linearly with the square root of the sweep rate, with the linear equation being Ipa(μA)=0.51855v1/2(mV s-1)1/22.75228, linear correlation coefficient 0.99851. In addition, when the sweep rate is increased, it is easy to cause instability of the base line, and 100mV s is selected for obtaining a larger peak current-1
7. Effect of enrichment time
And (3) dripping 6 mu L of AuNPs-ZnO-rGO dispersion liquid on the surfaces of a plurality of polished GCEs, and carrying out subsequent tests after the GCEs are dried.
Adding 6-Gingerol with the concentration of 100 mu M for testing, selecting the voltage range of 0.00-1.00V and the sweep rate of 100mV s-1The buffer solution was a pH2.0BR buffer solution, and CV test was performed. The enrichment step aims at pre-concentration and improves the detection sensitivity. This experiment mainly studied 6-Gingerol in AuNPs-Influence on the electrochemical behaviour of ZnO-rGO/GCE due to different enrichment times (t). The results of the experiment gave a line graph of 6-Gingerol in AuNPs-ZnO-rGO/GCE using cyclic voltammetry, as shown in FIG. 9. As t advances, the current increases, and at 120s, Ipa of 6-Gingerol on AuNPs-ZnO-rGO/GCE is basically stabilized, the peak position is 0.713V, and the Ipa is 3.029X 10-5A, which was then enriched, showed little change, and stabilized as seen in FIG. 9. Therefore, the enrichment time was set to 120s in subsequent experiments.
8. Influence of AuNPs-ZnO-rGO nano composite material dispersion liquid dosage
In this experiment, 3.0, 4.0, 5.0, 6.0, 7.0, 8.0, 9.0 μ L of AuNPs-ZnO-rGO dispersion was dropped on the polished GCE surface, and after waiting for drying, the subsequent experiment was performed. The concentration of 6-Gingerol was selected as 100. mu.M for the experiment. The applied voltage is 0.00-1.00V, the buffer solution is BR solution with pH value of 2.0 and sweep rate of 100mV s-1And t is 120s, and detection is performed by CV method. In the experiment, the influence of different amounts of the compound materials dripped on the modified electrode on current signals of 6-Gingerol in AuNPs-ZnO-rGO/GCE is mainly considered. From the results of the experiment, 6-Gingerol was prepared as a line graph at Ipa of AuNPs-ZnO-rGO/GCE. Referring to FIG. 10, it is clear that the Ipa for 6-Gingerol increases significantly as the AuNPs-ZnO-rGO dispersion dosage increases from 3. mu.L to 6. mu.L, and decreases between 6 and 9. mu.L, which is related to AuNPs-ZnO-rGO film thickness, with thicker film thicknesses and lower conductivity. So the experiment was modified on GCE with 6.0. mu.L of AuNPs-ZnO-rGO dispersion.
9. Determination of gingerol
In this experiment, 6.0 μ L of AuNPs-ZnO-rGO dispersion was dropped onto the polished GCE surface, and after drying, the subsequent tests were performed. Selecting 6-Gingerol with different concentrations for experiments, wherein the BR buffer solution with the applied voltage of 0.00-1.00V and the pH value of 2.0 has the sweep rate of 100mV s-1And t is 120s, and the LSV method is used for testing. The experiment was mainly examined for LSV response and corresponding linear calibration curves for different concentrations of 6-Gingerol, see FIG. 11 (A). As can be seen from FIG. 11(B), Ipa is linear with concentration c in the range of 0.1-100. mu.M, Ipa(μA)=0.44221c +1.86657(μ M), a linear correlation coefficient of 0.99421, and a LOD of 0.03 μ M (S/N — 3).
10. Selectivity, reproducibility and stability
To evaluate the selectivity of the developed electrochemical sensors, the effect of some possible interferents in the 6-Gingerol assay was evaluated. Under optimal experimental conditions, Ipa from 6-Gingerol recorded changes in the presence of interferents, respectively. FIG. 12 results show that Mg is 500 times the concentration2+,Ca2+,K+,Na+,SO42-,NO3-And 1000-fold concentration of glucose, dopamine, and ascorbic acid had no clear effect on the peak current of 30. mu.M 6-Gingerol (change in peak current)<5%)。
Reproducibility of the modified electrode was checked by 6 consecutive measurements of peak current response of 30 μ M6-Gingerol, with a Relative Standard Deviation (RSD) of 2.9%, indicating acceptable reproducibility, see FIG. 13.
Stability of modified electrode Ipa values of 30. mu.M 6-Gingerol were measured after two weeks by storing the modified electrode in a refrigerator at 4 ℃. The results show that only a small decrease in peak current is observed with a signal change of 3.9%, indicating that the AuNPs-ZnO-rGO/GCE has good stability.
11. Determination of actual samples
In the experiment, the potential window is selected to be 0.00-1.00V, the BR buffer solution with the pH value of 2.0, and the sweep rate is selected to be 100mV s-1And t is 120s, and the LSV method is used for testing. To facilitate the analysis of real samples, crushed ginger available on ginger was extracted from ginger. The sample weighed 1.0 g (unless otherwise stated) was poured into a centrifuge tube, 5mL of ethanol was used as a solvent, vigorously shaken with a vortex mixer for 1min, placed in an ultrasonic cleaner for 30min, and the mixture was centrifuged at 4000r/min for 10min to remove solids, and the supernatant was taken. The content of 6-Gingerol in ginger is determined by the same method as that for preparing a linear calibration chart, after the completion of the test, 6-Gingerol with a certain concentration is added for the determination of the recovery rate, and the recovery rate is determined in parallel for 5 times, and the experimental result can be used for preparing a curve chart of Ipa of 6-Gingerol on AuNPs-ZnO-rGO/GCE (figure 14). Curve a is the actual sampleThe LSV curve of 6-Gingerol in ginger on AuNPs-ZnO-rGO/GCE shows that the peak position is 0.676V, and the Ipa is 6.06 muA. The concentration of the actual sample was calculated to be 7.35. mu.M. Curves b, c, d, e, f are LSV plots of 6-Gingerol standard added dropwise at 10. mu.M, 20. mu.M, 30. mu.M, 50. mu.M, and 70. mu.M, respectively, and the peak positions are all around 0.673V. As can be seen from Table 1, this method was used to measure between 99.07% and 102.05%. Therefore, the accuracy and precision of the method are in accordance with the testing requirements.
TABLE 1 determination of 6-Gingerol in ginger samples using AuNPs-ZnO-rGO/GCE
Figure BDA0002403298820000091
aAverage of three determinations
In conclusion, the AuNPs-ZnO-rGO nano composite material is synthesized by an ultraviolet illumination method, the obtained AuNPs-ZnO-rGO nano composite material has good electrocatalysis effect on 6-Gingerol, the stability, the selectivity and the reproducibility are good, and the linear range of the concentration detection of 6-Gingerol is as follows: 0.1-100 mu M and LOD of 0.03 mu M (S/N is 3), and can be used for high-sensitivity and rapid determination of 6-Gingerol in ginger samples.

Claims (6)

1. An AuNPs-ZnO-rGO nano composite material synthesized by an ultraviolet light reduction method is characterized by comprising the following steps: step 1, weighing 5-10mg of graphene oxide, dispersing the graphene oxide in 20ml of ultrapure water, and performing ultrasonic treatment for 0.5-1h to obtain a GO dispersion solution; step 2, weighing 10-15mg of ZnO, dissolving in GO dispersion solution, carrying out ultrasonic treatment for 0.5-1h, and then adding 0.2-0.5mL of 0.0245M HAuCl4Carrying out ultrasonic treatment on the solution for 0.5-1h, and then irradiating the solution under an ultraviolet lamp for 20-30 minutes to obtain a mixture A; step 3, centrifuging the mixture A, and washing and precipitating with ultrapure water to obtain a nano composite material; the resulting nanocomposite was dispersed in ultrapure water and stored at 4 ℃ for use.
2. Use of AuNPs-ZnO-rGO nanocomposite prepared according to claim 1 in the preparation of an electrochemical sensor for detecting 6-gingerol.
3. The use of claim 2, wherein the electrolyte for detecting 6-gingerol is a BR solution.
4. The use of claim 2, wherein the pH of 6-gingerol is measured to be 2.
5. The use of claim 2, wherein the sweeping rate for detecting 6-gingerol is 100 mV.
6. The use according to claim 2, wherein the enrichment time for detecting 6-gingerol is 120 s.
CN202010153720.7A 2020-03-06 2020-03-06 AuNPs-ZnO-rGO nano composite material synthesized by ultraviolet illumination reduction method and application thereof Pending CN111272846A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010153720.7A CN111272846A (en) 2020-03-06 2020-03-06 AuNPs-ZnO-rGO nano composite material synthesized by ultraviolet illumination reduction method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010153720.7A CN111272846A (en) 2020-03-06 2020-03-06 AuNPs-ZnO-rGO nano composite material synthesized by ultraviolet illumination reduction method and application thereof

Publications (1)

Publication Number Publication Date
CN111272846A true CN111272846A (en) 2020-06-12

Family

ID=71003813

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010153720.7A Pending CN111272846A (en) 2020-03-06 2020-03-06 AuNPs-ZnO-rGO nano composite material synthesized by ultraviolet illumination reduction method and application thereof

Country Status (1)

Country Link
CN (1) CN111272846A (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20130344611A1 (en) * 2012-06-20 2013-12-26 Samsung Electronics Co., Ltd. Apparatus and method for analyzing graphene and graphene boundary
CN105092646A (en) * 2015-08-19 2015-11-25 电子科技大学 Graphene/metal oxide composite film gas sensor and preparation method
CN108931559A (en) * 2018-05-22 2018-12-04 山东大学 A kind of boron doping graphene modified Au@ZnO nucleocapsid heterojunction type triethylamine gas sensor and preparation method thereof
CN109248676A (en) * 2018-09-19 2019-01-22 福州大学 A kind of photocatalytic synthesis is at PbTiO3The method of/RGO composite material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20130344611A1 (en) * 2012-06-20 2013-12-26 Samsung Electronics Co., Ltd. Apparatus and method for analyzing graphene and graphene boundary
CN105092646A (en) * 2015-08-19 2015-11-25 电子科技大学 Graphene/metal oxide composite film gas sensor and preparation method
CN108931559A (en) * 2018-05-22 2018-12-04 山东大学 A kind of boron doping graphene modified Au@ZnO nucleocapsid heterojunction type triethylamine gas sensor and preparation method thereof
CN109248676A (en) * 2018-09-19 2019-01-22 福州大学 A kind of photocatalytic synthesis is at PbTiO3The method of/RGO composite material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
张金伟 等: "基于石墨烯复合材料电化学传感器的构建及性能研究", 《中国优秀博硕士学位论文全文数据库(硕士) 工程科技I辑》 *

Similar Documents

Publication Publication Date Title
Yang One-pot synthesis of reduced graphene oxide/zinc sulfide nanocomposite at room temperature for simultaneous determination of ascorbic acid, dopamine and uric acid
Fadeel et al. Adverse effects of engineered nanomaterials: exposure, toxicology, and impact on human health
Xu et al. Low-cost synthesis of carbon nanodots from natural products used as a fluorescent probe for the detection of ferrum (III) ions in lake water
Algarra et al. Enhanced electrochemical response of carbon quantum dot modified electrodes
Xu et al. Contribution of physicochemical characteristics of nano-oxides to cytotoxicity
Miao et al. Facile synthesis of carbon nanodots from ethanol and their application in ferric (III) ion assay
Tripathi et al. Pollutant soot of diesel engine exhaust transformed to carbon dots for multicoloured imaging of E. coli and sensing cholesterol
CN102142348B (en) Supporting membrane of transmission electron microscope sample and manufacturing method for transmission electron microscope sample
Liu et al. Preparation of nitrogen-doped carbon dots with high quantum yield from Bombyx mori silk for Fe (III) ions detection
Barhoum et al. Physicochemical characterization of nanomaterials: Size, morphology, optical, magnetic, and electrical properties
JP5370995B2 (en) Surface-enhanced Raman scattering reactive nanoscale pH sensor
Abdel-Haleem et al. t-Butyl calixarene/Fe2O3@ MWCNTs composite-based potentiometric sensor for determination of ivabradine hydrochloride in pharmaceutical formulations
Kong et al. UV-assisted photocatalytic synthesis of highly dispersed Ag nanoparticles supported on DNA decorated graphene for quantitative iodide analysis
Xiong et al. Catalyst-free synthesis of phenolic-resin-based carbon nanospheres for simultaneous electrochemical detection of Cu (II) and Hg (II)
Holbrook et al. Overview of nanomaterial characterization and metrology
CN107764788A (en) A kind of synthetic method of carbon quantum dot, carbon quantum dot and detection Fe3+Method
CN113552199B (en) FeS-based 2 Molecularly imprinted electrochemical sensor with/C/MQDs/GCE modified electrode and preparation method thereof
Rooyanian et al. A simple route to surface functionalization of graphene nanosheets by benzoic acid and its application toward Pb (ii) sensing
Shi et al. Co 2+ detection, cell imaging, and temperature sensing based on excitation-independent green-fluorescent N-doped carbon dots
Huan et al. Rational design of gold nanoparticle/graphene hybrids for simultaneous electrochemical determination of ascorbic acid, dopamine and uric acid
Li et al. A chemically reduced graphene oxide–Au nanocage composite for the electrochemical detection of dopamine and uric acid
Kingsford et al. Electrochemical sensing for 1-chloro-4-nitrobenzene based on β-cyclodextrin/carbon nanohorn nanohybrids
Patil et al. An update on sophisticated and advanced analytical tools for surface characterization of nanoparticles
Dang et al. Determination of norfloxacin using a tetraoxocalix [2] arene [2]-triazine covalently functionalized multi-walled carbon nanotubes modified electrode
Chen et al. Triangular gold nanoplates/two-dimensional nano mica platelets with a 3D lightning-rod effect as flexible nanohybrid substrates for SERS bacterial detection

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
CB02 Change of applicant information
CB02 Change of applicant information

Address after: 224051 Yancheng City hope road, Jiangsu, No. 1

Applicant after: YANCHENG INSTITUTE OF TECHNOLOGY

Address before: 224599 building, 1166 Century Avenue, Jiangsu, Yancheng City

Applicant before: YANCHENG INSTITUTE OF TECHNOLOGY

RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20200612