CN111337555A - Method for preparing reduced graphene oxide-nanogold composite material by using perilla extract and application of reduced graphene oxide-nanogold composite material in electrochemical sensor - Google Patents
Method for preparing reduced graphene oxide-nanogold composite material by using perilla extract and application of reduced graphene oxide-nanogold composite material in electrochemical sensor Download PDFInfo
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention belongs to the technical field of electrochemistry and nano materials, and provides a reduced graphene oxide-nano gold composite material prepared by using a perilla extract as a reducing agent, and the composite nano material is modified on the surface of an electrode and applied to high-sensitivity detection of electroactive substances. Firstly, preparing a perilla extract, then adding a chloroauric acid aqueous solution and a graphene oxide dispersion liquid into the obtained perilla extract, and heating the obtained mixed solution at 60 ℃ for 4 hours to obtain a black suspension; and cooling and filtering the suspension to obtain the green synthesized reduced graphene oxide-nano gold composite material. The invention adopts the perilla extract as a reducing agent and a stabilizing agent, has rich and easily obtained sources, mild reducing property and no harm to the environment; the composite material is modified on an electrode, and can be applied to high-sensitivity detection of electroactive substances.
Description
Technical Field
The invention belongs to the technical field of electrochemistry and nano materials, and provides a reduced graphene oxide-nano gold composite material prepared by using a perilla extract as a reducing agent, and the composite nano material is modified on the surface of an electrode and applied to high-sensitivity detection of electroactive substances.
Background
Graphene (Graphene) has a series of special properties such as perfect quantum tunneling effect, good thermal conductivity and conductivity effect and ultra-high specific surface area due to its unique monatomic structure, and has become an ideal electrode material for electrochemical sensors. The nano gold is gold material with the diameter of gold particles between 1 and 100nm, and is one of the most stable noble metal nano particles. The nano-gold is a very good conductive material, oxidized graphene and the nano-gold can be well infiltrated mutually, strong interaction exists, and the graphene-nano-gold composite material has potential wide application in the fields of catalysis and chemical sensors.
The key point for preparing the graphene-nano gold composite particles is to select a proper reducing agent. A plurality of preparation methods are reported at home and abroad, and most of the preparation methods need to adopt a chemical reducing agent, such as hydrazine hydrate (H)2NNH2·H2O), sodium tetrahydroborate (NaBH)4) Sodium citrate, etc., which have the problems of complicated conditions and environmental harm. The plant polyphenol becomes an ideal reducing agent and stabilizer for synthesizing the zero-valent nano-particles due to the advantages of abundant and easily-obtained sources, mild reducing property, no toxicity, no harm and the like.
Perilla frutescens L is a traditional plant used as both medicine and food, and the leaves of Perilla frutescens L contain abundant polyphenols such as catechin, ferulic acid, apigenin, luteolin and caffeic acid. There are many patents which adopt tea leaves or tea leaf extracts to synthesize nano-gold, nano-silver or nano-copper nano-particles; the perilla contains rich polyphenol, the source is rich and easy to obtain, the reduction property of the perilla extracting solution is mild, and the perilla extracting solution has no harm to the environment, so that the perilla becomes an ideal reducing agent and stabilizer for synthesizing nano particles. The invention belongs to the technical field of electrochemistry and nano materials, and relates to a green controllable preparation method of a reduced graphene oxide-nano gold composite material, wherein the composite nano material is modified on the surface of an electrode and is applied to high-sensitivity detection of electroactive substances.
Disclosure of Invention
One object of the present invention is to prepare a reduced graphene oxide-nanogold composite material based on a perilla extract as a reducing agent;
another object of the present invention is to provide a method for preparing the graphene-nanogold composite material; the preparation method is environment-friendly, mild in reaction condition, simple in process and low in cost, and the obtained composite material has good electrocatalytic performance and can be applied to high-sensitivity detection of electroactive substances.
In order to achieve the purpose, the invention adopts the following technical means:
the preparation method of the reduced graphene oxide-nanogold composite material based on the perilla frutescens extract as the reducing agent comprises the following specific steps:
(1) weighing 10.0 g of perilla leaf, adding 100mL of ethanol and distilled water according to the volume ratio of 1: 1, carrying out ultrasonic extraction for 2 hours in the dark, filtering by a 0.22 mu m polypropylene film to obtain a perilla extract, and storing the filtrate in a refrigerator at 4 ℃ in the dark;
(2) adding graphene oxide into 10mL of distilled water, and performing ultrasonic treatment for 30min to form a uniform dispersion liquid;
(3) adding tetrachloroauric acid into 10mL of distilled water to obtain chloroauric acid aqueous solution;
(4) adding the tetrachloroauric acid aqueous solution and the graphene oxide dispersion liquid into the perilla frutescens extract obtained in the step (1),
(5) heating the mixed solution obtained in the step (4) at 60 ℃ for 4 hours to obtain a black suspension;
(6) after the suspension is cooled, carrying out suction filtration, washing with distilled water and absolute ethyl alcohol, putting into a vacuum drying oven for drying for 6-8h at the temperature of 60 ℃, and grinding to obtain a green synthesized reduced graphene oxide-nanogold composite material;
further, the mass ratio of the graphene oxide and the tetrachloroauric acid in the mixed solution is 1: 1.
furthermore, the volume ratio of the perilla extract to the graphene dispersion liquid to the tetrachloroauric acid aqueous solution is 2:1 respectively.
The invention also aims to modify the graphene-nano gold composite material on the surface of an electrode, and apply the graphene-nano gold composite material to high-sensitivity detection of electroactive substancesThe method comprises the following steps: 5 mg of reduced graphene oxide-nanogold composite material is added into 5mLN， NDimethylformamide, then sonicated for 30 minutes to form a uniform dispersion. 10 uL of the dispersion liquid is transferred by a liquid transfer gun and is coated on a glassy carbon electrode which is polished into a mirror surface, and the glassy carbon electrode is naturally dried at room temperature.
Further, the electrode prepared above was used as a working electrode, Ag/AgCl as a reference electrode, a platinum wire as a counter electrode, and 0.05 mol L of the counter electrode was used-1The electrode was subjected to differential pulse scanning (DPV) in different concentrations of folic acid solution as a buffer solution (pH = 7.0). The peak current of the DPV spectrum is increased along with the increase of the concentration of folic acid, and the peak current at the potential of-0.700 is selected for quantitative analysis.
Compared with the existing preparation method of the reduced graphene oxide-nano gold composite material, the preparation method has the advantages that: 1. the perilla extract is used as a reducing agent and a stabilizing agent, and has the advantages of abundant and easily-obtained sources, mild reducing property and no harm to the environment; 2. the composite material is modified on an electrode, and can be applied to high-sensitivity detection of electroactive substances.
Drawings
FIG. 1 shows the polyphenols apigenin (apigenin), luteolin (luteolin), catechin ((+) catechin), caffeic acid (caffeic acid) and ferulic acid (ferulic acid) contained in the leaves of Perilla frutescens.
FIG. 2 is a TEM image of a reduced graphene oxide-nanogold composite prepared by the invention;
FIG. 3 is an XRD pattern of a reduced graphene oxide-nanogold composite material prepared by the invention;
FIG. 4 is a DPV graph of folic acid of different concentrations on a reduced graphene oxide-nanogold composite material (the concentrations of folic acid are respectively 0.02, 0.04, 0.08, 0.12, 0.2, 0.4, 0.8, 2, 4, 5, 8 and 10 [ mu ] mol L from bottom to top)-1；
FIG. 5 is a linear relationship of DPV peak current of folate to folate concentration;
FIG. 6 is a linear relationship of DPV peak current of folate to folate concentration (low concentration).
Detailed Description
Example 1
Preparation of Perilla extract
Accurately weighing 10.0 g of perilla leaf (dried), grinding, adding 100ml of mixed solution of ethanol and water (volume ratio of 1: 1), ultrasonically extracting for 2 hours in the dark, filtering through a 0.22 μm polypropylene film, and storing the filtrate in the dark at 4 ℃. The perilla contains rich polyphenol, which contains both water-soluble components and fat-soluble components, and the mixed solution of ethanol and water is helpful for extracting the polyphenol. The structure of polyphenols contained in Perillae herba as reducing agent is shown in figure 1.
Preparation of reduced graphene oxide-nanogold composite material
Adding 0.5g of graphene oxide into 10mL of distilled water, and carrying out ultrasonic treatment for 30min to form a uniform dispersion liquid; about 0.5g of tetrachloroauric acid was added to 10mL of distilled water to obtain an aqueous chloroauric acid solution. Adding the chloroauric acid aqueous solution and the graphene oxide dispersion liquid into 20mL of filtered perilla extract, and heating the obtained mixed solution at 60 ℃ for 4 hours to obtain a black suspension; and cooling and filtering the suspension, washing the suspension with deionized water and absolute ethyl alcohol, drying the suspension in a vacuum drying oven at the temperature of 60 ℃ for 6-8h, and grinding the dried suspension to obtain the green synthesized reduced graphene oxide-nanogold composite material.
Characterization of reduced graphene oxide-nanogold composites
Fig. 2 is a Transmission Electron Microscope (TEM) of the reduced graphene-nanogold composite material prepared by the present invention, wherein it can be seen that the gold nanoparticles are uniformly distributed on the sheet-shaped graphene, and the average diameter of the obtained gold nanoparticles is about 20 nm. Fig. 3 is an X-ray diffraction pattern (XRD) of the reduced graphene-nanogold composite prepared according to the present invention. It can be seen that the 4 diffraction peaks appearing at 8.25, 44.21, 64.71 and 77.54 of 2 θ are characteristic diffraction peaks of gold, corresponding to the face-centered cubic (FCC) structure A u (111), (200), (220) and (311) crystal planes, respectively; meanwhile, the characteristic peak of graphene oxide (curve a) 2 θ at 11.16 disappears on curve b, thereby determining that the product is reduced graphene oxide-nanogold.
Application example 1
Application of reduced graphene oxide-nanogold composite material to modification of electrode
1 mg of reduced graphene oxide-nanogold composite material is added into 1 mLN，NDimethylformamide, then sonicated for 30 minutes to form a uniform dispersion. 10 uL of the dispersion liquid is transferred and coated on a glassy carbon electrode which is polished into a mirror surface, and the glassy carbon electrode is naturally dried at room temperature.
Example 5 determination of electroactive substance folic acid by reduced graphene oxide-nanogold composite
The electrode prepared above is used as a working electrode, Ag/AgCl is used as a reference electrode, a platinum wire is used as a counter electrode, and 0.05 mol L of the electrode is used-1The phosphate buffer solution (pH = 7.0) as a buffer solution, the electrode was subjected to differential pulse scanning (DPV) in folic acid solutions of different concentrations, the scanning potential ranges were: 1.0-0V, and figure 4 is the scanning spectrum obtained. The peak current of the DPV spectrum is increased along with the increase of the concentration of folic acid, and the peak current at the potential of-0.700 is selected for quantitative analysis. When the concentration of folic acid is 0.02-0.8 mu mol L-1And 0.8-10. mu. mol L-1When in the range, the DPV peak current is linear with concentration. When the concentration is 0.02-0.8 mu mol L-1In the range, I (mu A) = 6.95985c (mu mol L)-1) + 1.27538, correlation coefficient R = 0.9930 (fig. 5); when the concentration is 0.8-10 mu mol L-1In the range, I (mu A) = 0.75627c (mu molL)-1) + 5.79855, correlation coefficient R = 0.9944 (FIG. 6), detection limit of 2.8 nmol.L-1(S/N=3)。
Claims (7)
1. A method for preparing a reduced graphene oxide-nanogold composite material by using a perilla extract is characterized in that,
firstly, preparing a perilla extract, then adding a chloroauric acid aqueous solution and a graphene oxide dispersion liquid into the obtained perilla extract, heating the obtained mixed solution to obtain a black suspension, cooling and then carrying out suction filtration to obtain the reduced graphene oxide-nanogold composite material.
2. The method for preparing a reduced graphene oxide-nanogold composite material using a perilla extract according to claim 1, comprising the steps of:
(1) weighing 10.0 g of perilla leaf, adding 100mL of ethanol and distilled water according to the volume ratio of 1: 1, carrying out ultrasonic extraction for 2 hours in the dark, filtering by a 0.22 mu m polypropylene film to obtain a perilla extract, and storing the filtrate in a refrigerator at 4 ℃ in the dark;
(2) adding graphene oxide into 10mL of distilled water, and performing ultrasonic treatment for 30min to form a uniform dispersion liquid;
(3) adding tetrachloroauric acid into 10mL of distilled water to obtain chloroauric acid aqueous solution;
(4) adding the tetrachloroauric acid aqueous solution and the graphene oxide dispersion liquid into the perilla frutescens extract obtained in the step (1),
(5) heating the mixed solution obtained in the step (4) at 60 ℃ for 4 hours to obtain a black suspension;
(6) and after cooling the suspension, carrying out suction filtration, washing with distilled water and absolute ethyl alcohol, drying in a vacuum drying oven at 60 ℃ for 6-8h, and grinding to obtain the green synthesized reduced graphene oxide-nanogold composite material.
3. The method of claim 2, wherein the mass ratio of the graphene oxide to the tetrachloroauric acid in the mixed solution is 1: 1.
4. the method according to claim 2, wherein the volume ratio of the perilla herb extract to the graphene dispersion and the tetrachloroauric acid aqueous solution is 2:1, respectively.
5. The application of the reduced graphene oxide-nano gold composite material prepared by the method of any one of claims 1 to 4 in an electrochemical sensor.
6. Use according to claim 5, characterized in that: the composite gold nano material is applied to the detection of folic acid, and the detection method comprises the following steps:
(1) 5 mg of reduced graphene oxide-nanogold composite material is added into 5mLN，NDimethyl formamide, and then carrying out ultrasonic treatment to form a uniform dispersion liquid;
(2) 10 uL of dispersion liquid is transferred and coated on a glassy carbon electrode which is polished into a mirror surface, and natural drying is carried out at room temperature;
(3) the electrode prepared above was used as a working electrode, Ag/AgCl as a reference electrode, a platinum wire as a counter electrode, and a wire containing 0.05 mol L-1pH =7.0 phosphate buffer as buffer solution, the electrodes were differentially pulse scanned DPV in different concentrations of folic acid solution,
(4) the peak current of the DPV spectrum is increased along with the increase of the concentration of folic acid, and the peak current at the potential of-0.700 is selected for quantitative analysis.
7. The use of claim 5, wherein said folic acid of step (3) comprises one of folic acid, dopamine, ascorbic acid.
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| CN114950411A (en) * | 2022-06-30 | 2022-08-30 | 中国科学技术大学 | Noble metal single-atom catalyst, preparation method thereof and application thereof in ascorbic acid detection |
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Application publication date: 20200626 |