CN110057891B - Preparation method and application of PtCu RNDFs-based electrochemical sensor - Google Patents
Preparation method and application of PtCu RNDFs-based electrochemical sensor Download PDFInfo
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- CN110057891B CN110057891B CN201910329093.5A CN201910329093A CN110057891B CN 110057891 B CN110057891 B CN 110057891B CN 201910329093 A CN201910329093 A CN 201910329093A CN 110057891 B CN110057891 B CN 110057891B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 238000001514 detection method Methods 0.000 claims abstract description 49
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 38
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 38
- 229930195730 Aflatoxin Natural products 0.000 claims abstract description 30
- 239000005409 aflatoxin Substances 0.000 claims abstract description 30
- XWIYFDMXXLINPU-UHFFFAOYSA-N Aflatoxin G Chemical compound O=C1OCCC2=C1C(=O)OC1=C2C(OC)=CC2=C1C1C=COC1O2 XWIYFDMXXLINPU-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 15
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- OQIQSTLJSLGHID-WNWIJWBNSA-N aflatoxin B1 Chemical compound C=1([C@@H]2C=CO[C@@H]2OC=1C=C(C1=2)OC)C=2OC(=O)C2=C1CCC2=O OQIQSTLJSLGHID-WNWIJWBNSA-N 0.000 claims description 6
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- -1 potassium ferricyanide Chemical compound 0.000 claims description 6
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 5
- GIAFURWZWWWBQT-UHFFFAOYSA-N 2-(2-aminoethoxy)ethanol Chemical compound NCCOCCO GIAFURWZWWWBQT-UHFFFAOYSA-N 0.000 claims description 5
- 229930063498 Aflatoxin G1 Natural products 0.000 claims description 5
- XWIYFDMXXLINPU-WNWIJWBNSA-N Aflatoxin G1 Chemical compound O=C1OCCC2=C1C(=O)OC1=C2C(OC)=CC2=C1[C@@H]1C=CO[C@@H]1O2 XWIYFDMXXLINPU-WNWIJWBNSA-N 0.000 claims description 5
- 108091003079 Bovine Serum Albumin Proteins 0.000 claims description 5
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 239000002098 aflatoxin G1 Substances 0.000 claims description 5
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- 229910052786 argon Inorganic materials 0.000 claims description 5
- 229940098773 bovine serum albumin Drugs 0.000 claims description 5
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 5
- MPTQRFCYZCXJFQ-UHFFFAOYSA-L copper(II) chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Cu+2] MPTQRFCYZCXJFQ-UHFFFAOYSA-L 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 5
- 238000005530 etching Methods 0.000 claims description 5
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- 239000005457 ice water Substances 0.000 claims description 5
- 239000004005 microsphere Substances 0.000 claims description 5
- PDKHNCYLMVRIFV-UHFFFAOYSA-H molybdenum;hexachloride Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Mo] PDKHNCYLMVRIFV-UHFFFAOYSA-H 0.000 claims description 5
- 239000005543 nano-size silicon particle Substances 0.000 claims description 5
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- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
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- KLFRPGNCEJNEKU-FDGPNNRMSA-L (z)-4-oxopent-2-en-2-olate;platinum(2+) Chemical compound [Pt+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O KLFRPGNCEJNEKU-FDGPNNRMSA-L 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 3
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 3
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 3
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- B82Y40/00—Manufacture or treatment of nanostructures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention belongs to the technical field of immunoassay and biosensing, and provides a preparation method and application of an electrochemical sensor based on PtCu RNDFs. The invention uses N-MoS2QDs @ MWCNTs are used as a substrate material, and the excellent conductivity, large specific surface area and high catalytic activity of the QDs @ MWCNTs can effectively reduce background signals; meanwhile, PtCuRNDFs and detection antibody incubation are used as signal markers to further enhance the catalytic performance and amplify signals of the electrochemical sensor, so that the quantitative detection of the aflatoxin is realized, and the method has the advantages of low detection limit, high sensitivity, good repeatability, selectivity, stability and the like, and has important scientific significance and application value for detecting the aflatoxin.
Description
Technical Field
The invention belongs to the technical field of immunoassay, nano materials and biosensing, and provides a preparation method and application of an electrochemical sensor based on PtCuRNDFs.
Background
In recent years, food pollution is becoming more serious and frequent, and the health of human beings is seriously threatened while huge economic losses are caused. Aflatoxins exist in soil, animals, plants and various nuts, are particularly easy to pollute grain and oil products such as peanuts, corns, rice, soybeans, wheat and the like, and are mycotoxins which have the highest mycotoxin poisoning property and extremely obvious harm to human health. Due to wide distribution, the feed easily enters a food chain through polluted grains or feeds and the like, further pollutes animal-derived foods such as milk, eggs, meat and the like, and indirectly enters a human body, and finally serious consequences such as liver and kidney injury, reproductive disorder, immunosuppression, carcinogenesis and teratogenesis are caused.
At present, the aflatoxin detection method comprises a thin layer analysis method, a liquid chromatography method, a fluorescence photometry method, an enzyme linked immunosorbent assay, a capillary electrophoresis method, an electrochemical immunoassay method and the like. Wherein, the thin-layer analysis method has complex and time-consuming operation, unsatisfactory extraction and purification effects and poor sensitivity; the liquid chromatography instrument is expensive, and the pretreatment method is relatively complex; the fluorescence photometry has higher detection cost, needs to be provided with special equipment and cannot detect single toxin; the enzyme-linked immunoassay has poor repeatability, short reagent life, low-temperature storage and higher false positive probability; the capillary electrophoresis method has high cost and complex operation, and is not suitable for being widely applied to sample detection; the electrochemical immunoassay method has the advantages of high selectivity, quick response, simple operation, convenient carrying, suitability for field detection and the like, so researchers are actively exploring and developing a novel electrochemical sensor for detecting aflatoxin.
The invention successfully constructs an electrochemical sensor based on PtCuRNDFs, and the base material of the sensor is N-MoS2QDs @ MWCNTs, wherein N-MoS2QDs not only have good electrocatalytic activity but also have strong electrical conductivity; the multi-wall carbon nano-tube has large specific surface area and strong conductivity, and can load a large amount of N-MoS after carboxylation2QDs and capture antibody Ab1。PtCu RNDFs is used as a detection antibody marker, the sensitivity of the immunosensor can be increased, the catalytic activity can be further improved, the further amplification of a detection signal can be realized, and meanwhile, the structure of the PtCu alloy dodecahedral nano-framework has a large specific surface area and can load a large amount of detection antibody Ab2. The invention adopts N-MoS2The QDs @ MWCNTs is used as a substrate material, and the PtCu RNDFs are used as an electrochemical sensor constructed for detecting antibody markers, so that the aflatoxin detection is realized, the detection limit is low, the sensitivity is high, the acceptable repeatability, the selectivity and the stability are realized, and the important scientific significance and the application value are realized for the aflatoxin detection.
Disclosure of Invention
The invention provides a preparation method and application of an electrochemical sensor based on PtCu RNDFs, which realize sensitive detection of aflatoxin.
The invention aims to provide a preparation method of an electrochemical sensor based on PtCu RNDFs.
The other purpose of the invention is to apply the prepared PtCu RNDFs-based electrochemical sensor to the high-sensitivity and specific detection of aflatoxin.
The technical scheme of the invention comprises the following steps.
1. A preparation method of an electrochemical sensor based on PtCu RNDFs comprises the following steps:
(1) al for glassy carbon electrode with diameter of 4 mm2O3Polishing the polishing powder into a mirror surface, and cleaning with ultrapure water;
(2) N-MoS of 6 muL and 1.0-3.0 mg/mL2Dripping QDs @ MWCNTs solution on the surface of the electrode, drying at room temperature, washing the surface of the electrode with ultrapure water, and drying;
(3) continuing to capture the aflatoxin capture antibody Ab of 6 muL and 8-12 mug/mL1Dropwise adding the solution to the surface of an electrode, washing with ultrapure water, and drying in a refrigerator at 4 ℃;
(4) continuously dropwise adding bovine serum albumin BSA solution with the mass fraction of 1% to the surface of the electrode by 3 muL, 0.5-1.5 mg/mL to seal non-specific active sites on the surface of the electrode, washing the surface of the electrode with ultrapure water, removing unbound BSA, and drying in a refrigerator at 4 ℃;
(5) continuously dropwise adding a series of aflatoxin antigen solutions with different concentrations, namely 6 muL and 10 pg/mL-100 ng/mL, washing the surface of the electrode with ultrapure water, and airing in a refrigerator at 4 ℃;
(6) continuously dropwise adding the detection antibody hatching substance PtCu RNDFs-Ab of 6 muL and 1.5-3.5 mg/mL2 And putting the solution on the surface of an electrode, incubating for 40 min in a refrigerator at 4 ℃, washing with ultrapure water, and airing to prepare the PtCuRNDFs-based electrochemical sensor.
2.N-MoS2The preparation method of the QDs @ MWCNTs solution comprises the following steps:
（1）N-MoS2preparation of QDs
Respectively weighing 0.2-0.7 g of molybdenum chloride and 1.0-3.0 g of thiourea, uniformly mixing, slowly adding 10 mL of ethanol, and stirring; after complete dissolution, continuously adding 2.0-4.0 g of nano silicon dioxide microspheres, carrying out ultrasonic treatment for 30 min, and drying at room temperature; then heating the mixture for 2-4 hours at 650 ℃ in a tubular furnace under the protection of argon; etching the obtained product with 30 mL of 5 mol/L sodium hydroxide for 24 h, and centrifugally cleaning the product for three times with ultrapure water to obtain the N-MoS2；
The N-MoS prepared above was added to 200 mL of N, N-dimethylformamide2 100 mg, ultrasonically treating in ice-water bath for 3 h, centrifuging at 3000 rpm for 10 min to obtain N-MoS2QDs；
（2）N-MoS2Preparation of QDs @ MWCNTs
Adding 10-30 mL of N-MoS into 25 mL and 1 mg/mL of carboxylated multi-walled carbon nano-tubes2QDs, stirring for 4 h after ultrasonic dispersion, centrifugally cleaning for three times by ultrapure water, and drying for 10 h in vacuum at 60 ℃ to obtain N-MoS2QDs@MWCNTs。
3. Detection of antibody hatchlings PtCu RNDFs-Ab2The solution was prepared by the following steps:
(1) preparation of PtCu RNDFs
Adding 0.25-3.0 g of hexadecyl trimethyl ammonium chloride into 30.0-40.0 mL of oleylamine, uniformly mixing, sequentially adding 0.02-0.04 g of platinum diacetylacetonate, 0.012 g of copper chloride dihydrate and 80-90 mu L of diglycolamine, and performing ultrasonic treatment for 20 min; transferring to a polytetrafluoroethylene-lined stainless steel reaction kettle, heating at 180 ℃ for reaction for 8-12 h, centrifugally cleaning the obtained product with an ethanol/cyclohexane 10:1 mixture for three times, and drying in vacuum at 60 ℃ to obtain PtCuRNDFs;
(2) detection of antibody hatchlings PtCu RNDFs-Ab2Preparation of the solution
Adding 1-3 mL of PtCu RNDFs solution with the concentration of 2 mg/mL into 0.5-1.5 mL of aflatoxin detection antibody solution Ab with the concentration of 10 mu g/mL2Performing shake incubation for 12 h in a constant temperature shaking box at 4 ℃, centrifuging and washing, adding into 1-3 mL of phosphoric acid buffer solution with pH = 7.38 to prepare the antibody hatching substance PtCuRNDFs-Ab for detection2The solution was stored at 4 ℃ until use.
4. Detecting aflatoxin by the following steps:
(1) testing by using an electrochemical workstation in a three-electrode system, taking a saturated calomel electrode as a reference electrode, taking a platinum wire electrode as an auxiliary electrode, taking the prepared sensor as a working electrode, and testing in 10 mL of potassium ferricyanide solution containing 10 mmol/L;
(2) detecting aflatoxin by a time-lapse current method, selecting-0.4V as the detection of current measurement, wherein the input voltage is-0.4V, the sampling interval is 0.1 s, and the running time is 300 s;
(3) when the background current tended to be stable, 10 μ L of 5 mol/L hydrogen peroxide solution was injected into 10 mL of 50 mmol/L phosphate buffer solution with pH = 7.38 every 50 s, and the change in current was recorded.
5. The detection of aflatoxins is selected from one of the following: aflatoxin B1, aflatoxin G1.
The raw materials used in the present invention are all available from chemical agents companies or biopharmaceutical companies.
Advantageous results of the invention
(1) The substrate material used in the invention is N-MoS2QDs @ MWCNTs, wherein N-MoS2QDs vs MoS2On one hand, the surface of the catalyst has abundant active sites due to the reduction of the size, so that the catalytic activity is improved; second, chemical doping makes the material conductiveFurther improvement is achieved; the multi-wall carbon nano-tube has large specific surface area and good conductivity, and can load a large amount of N-MoS after carboxylation2QDs and capture antibody Ab1The combination of the base materials enables the respective advantages to be better exerted. The PtCu RNDFs are used as detection antibody markers, so that the sensitivity of the electrochemical sensor can be increased, the catalytic activity of the electrochemical sensor can be improved, and the detection signal can be further amplified. The PtCu RNDFs are dodecahedral nano-frameworks, and the special interconnection corners and highly open structures of the PtCu RNDFs provide rich active sites and a large specific surface, and have good physical properties and chemical stability. The invention adopts N-MoS2The QDs @ MWCNTs is used as a substrate material, and the PtCu RNDFs are used as an electrochemical sensor constructed by detecting antibody markers, so that the aflatoxin can be sensitively and quickly detected.
(2) The electrochemical sensor based on the PtCu RNDFs realizes detection of aflatoxin, the linear range of the electrochemical sensor is 10 pg-60 ng/mL, and the detection limit is 3.33 pg/mL, so that the aim of accurate determination can be fulfilled by the electrochemical sensor based on the PtCu RNDFs.
Detailed Description
The present invention will now be further illustrated by, but not limited to, specific embodiments thereof.
Embodiment 1 a method for preparing an electrochemical sensor based on PtCu RNDFs, comprising the steps of:
(1) al for glassy carbon electrode with diameter of 4 mm2O3Polishing the polishing powder into a mirror surface, and cleaning with ultrapure water;
(2) N-MoS of 6 mu L and 1.0 mg/mL2Dripping QDs @ MWCNTs solution on the surface of the electrode, drying at room temperature, washing the surface of the electrode with ultrapure water, and drying;
(3) continuing to capture 6 muL and 8 mug/mL aflatoxin-captured antibody Ab1Dropwise adding the solution to the surface of an electrode, washing with ultrapure water, and drying in a refrigerator at 4 ℃;
(4) continuously dropwise adding bovine serum albumin BSA solution with the mass fraction of 1% to the surface of the electrode by 3 muL and 0.5 mg/mL to seal non-specific active sites on the surface of the electrode, washing the surface of the electrode with ultrapure water, removing unbound BSA, and drying in a refrigerator at 4 ℃;
(5) continuously dropwise adding a series of aflatoxin antigen solutions with different concentrations, namely 6 muL and 10 pg/mL-60 ng/mL, washing the surface of the electrode with ultrapure water, and airing in a refrigerator at 4 ℃;
(6) continuously dropwise adding detection antibody hatching material PtCu RNDFs-Ab of 6 mu L and 1.5 mg/mL2And putting the solution on the surface of an electrode, incubating for 40 min in a refrigerator at 4 ℃, washing with ultrapure water, and airing to prepare the PtCuRNDFs-based electrochemical sensor.
Embodiment 2 a method for manufacturing an electrochemical sensor based on PtCu RNDFs, comprising the steps of:
(1) al for glassy carbon electrode with diameter of 4 mm2O3Polishing the polishing powder into a mirror surface, and cleaning with ultrapure water;
(2) N-MoS of 6 mu L and 2.0 mg/mL2Dripping QDs @ MWCNTs solution on the surface of the electrode, drying at room temperature, washing the surface of the electrode with ultrapure water, and drying;
(3) continuing to capture the aflatoxin capture antibody Ab at 6 muL and 10 mug/mL1Dropwise adding the solution to the surface of an electrode, washing with ultrapure water, and drying in a refrigerator at 4 ℃;
(4) continuously dropwise adding bovine serum albumin BSA solution with the mass fraction of 1% to the surface of the electrode by 3 muL and 1.0 mg/mL to seal non-specific active sites on the surface of the electrode, washing the surface of the electrode with ultrapure water, removing unbound BSA, and drying in a refrigerator at 4 ℃;
(5) continuously dropwise adding a series of aflatoxin antigen solutions with different concentrations, namely 6 muL and 10 pg/mL-60 ng/mL, washing the surface of the electrode with ultrapure water, and airing in a refrigerator at 4 ℃;
(6) continuously dropwise adding detection antibody hatching material PtCu RNDFs-Ab of 6 mu L and 2.5 mg/mL2And putting the solution on the surface of an electrode, incubating for 40 min in a refrigerator at 4 ℃, washing with ultrapure water, and airing to prepare the PtCuRNDFs-based electrochemical sensor.
Embodiment 3 a method for manufacturing an electrochemical sensor based on PtCu RNDFs, comprising the steps of:
(1) will have a diameter of4 mm of Al for glassy carbon electrode2O3Polishing the polishing powder into a mirror surface, and cleaning with ultrapure water;
(2) N-MoS of 6 mu L and 3.0 mg/mL2Dripping QDs @ MWCNTs solution on the surface of the electrode, drying at room temperature, washing the surface of the electrode with ultrapure water, and drying;
(3) continuing to capture the aflatoxin capture antibody Ab at 6 muL and 12 mug/mL1Dropwise adding the solution to the surface of an electrode, washing with ultrapure water, and drying in a refrigerator at 4 ℃;
(4) continuously dropwise adding bovine serum albumin BSA solution with the mass fraction of 1% to the surface of the electrode by 3 muL and 1.5 mg/mL to seal non-specific active sites on the surface of the electrode, washing the surface of the electrode with ultrapure water, removing unbound BSA, and drying in a refrigerator at 4 ℃;
(5) continuously dropwise adding a series of aflatoxin antigen solutions with different concentrations, namely 6 muL and 10 pg/mL-60 ng/mL, washing the surface of the electrode with ultrapure water, and airing in a refrigerator at 4 ℃;
(6) continuously dropwise adding detection antibody hatching material PtCu RNDFs-Ab of 6 mu L and 3.5 mg/mL2And putting the solution on the surface of an electrode, incubating for 40 min in a refrigerator at 4 ℃, washing with ultrapure water, and airing to prepare the PtCuRNDFs-based electrochemical sensor.
Example 4N-MoS2The preparation method of the QDs @ MWCNTs solution comprises the following steps:
（1）N-MoS2preparation of QDs
Respectively weighing 0.2 g of molybdenum chloride and 1.0 g of thiourea, uniformly mixing, slowly adding 10 mL of ethanol, and stirring; after complete dissolution, 2.0 g of nano silicon dioxide microspheres are continuously added, and the mixture is dried at room temperature after ultrasonic treatment for 30 min; then heating for 2 h at 650 ℃ in a tube furnace under the protection of argon; etching the obtained product with 30 mL of 5 mol/L sodium hydroxide for 24 h, and centrifugally cleaning the product for three times with ultrapure water to obtain the N-MoS2；
The N-MoS prepared above was added to 200 mL of N, N-dimethylformamide2 100 mg, ultrasonically treating in ice-water bath for 3 h, centrifuging at 3000 rpm for 10 min to obtain N-MoS2QDs；
（2）N-MoS2Preparation of QDs @ MWCNTs
Adding 10 mL of N-MoS into 25 mL and 1 mg/mL carboxylated multi-wall carbon nano-tubes2QDs, stirring for 4 h after ultrasonic dispersion, centrifugally cleaning for three times by ultrapure water, and drying for 10 h in vacuum at 60 ℃ to obtain N-MoS2QDs@MWCNTs。
Example 5N-MoS2The preparation method of the QDs @ MWCNTs solution comprises the following steps:
（1）N-MoS2preparation of QDs
Respectively weighing 0.5 g of molybdenum chloride and 2.0 g of thiourea, uniformly mixing, slowly adding 10 mL of ethanol, and stirring; after complete dissolution, continuously adding 3.0 g of nano silicon dioxide microspheres, carrying out ultrasonic treatment for 30 min, and drying at room temperature; then heating for 3 hours at 650 ℃ in a tube furnace under the protection of argon; etching the obtained product with 30 mL of 5 mol/L sodium hydroxide for 24 h, and centrifugally cleaning the product for three times with ultrapure water to obtain the N-MoS2；
The N-MoS prepared above was added to 200 mL of N, N-dimethylformamide2 100 mg, ultrasonically treating in ice-water bath for 3 h, centrifuging at 3000 rpm for 10 min to obtain N-MoS2QDs；
（2）N-MoS2Preparation of QDs @ MWCNTs
20 mL of N-MoS was added to 25 mL of 1 mg/mL carboxylated multiwalled carbon nanotube2QDs, stirring for 4 h after ultrasonic dispersion, centrifugally cleaning for three times by ultrapure water, and drying for 10 h in vacuum at 60 ℃ to obtain N-MoS2QDs@MWCNTs。
Example 6N-MoS2The preparation method of the QDs @ MWCNTs solution comprises the following steps:
（1）N-MoS2preparation of QDs
Respectively weighing 0.7 g of molybdenum chloride and 3.0 g of thiourea, uniformly mixing, slowly adding 10 mL of ethanol, and stirring; after complete dissolution, continuously adding 4.0 g of nano silicon dioxide microspheres, carrying out ultrasonic treatment for 30 min, and then drying at room temperature; then heating for 4 hours at 650 ℃ in a tube furnace under the protection of argon; etching the obtained product with 30 mL of 5 mol/L sodium hydroxide for 24 h, and centrifugally cleaning the product for three times with ultrapure water to obtain the N-MoS2；
The N-MoS prepared above was added to 200 mL of N, N-dimethylformamide2 100 mg, ultrasonically treating in ice-water bath for 3 h, centrifuging at 3000 rpm for 10 min to obtain N-MoS2QDs；
（2）N-MoS2Preparation of QDs @ MWCNTs
Adding 30 mL of N-MoS into 25 mL and 1 mg/mL carboxylated multi-wall carbon nano-tubes2QDs, stirring for 4 h after ultrasonic dispersion, centrifugally cleaning for three times by ultrapure water, and drying for 10 h in vacuum at 60 ℃ to obtain N-MoS2QDs@MWCNTs。
Example 7 detection of antibody hatchlings PtCu RNDFs-Ab2The solution was prepared by the following steps:
(1) preparation of PtCu RNDFs
Adding 0.25 g of hexadecyl trimethyl ammonium chloride into 30 mL of oleylamine, uniformly mixing, sequentially adding 0.02 g of platinum diacetyl acetonate, 0.012 g of copper chloride dihydrate and 80 muL of diglycolamine, and carrying out ultrasonic treatment for 20 min; transferring to a stainless steel reaction kettle with a polytetrafluoroethylene lining, heating at 180 ℃ for 8 h, centrifugally cleaning the obtained product with an ethanol/cyclohexane 10:1 mixture for three times, and drying in vacuum at 60 ℃ to obtain PtCuRNDFs;
(2) detection of antibody hatchlings PtCu RNDFs-Ab2Preparation of the solution
1 mL of the PtCu RNDFs solution at a concentration of 2 mg/mL was added to 0.5 mL of the aflatoxin-detecting antibody solution Ab at a concentration of 10. mu.g/mL2In the step (b), the cells are incubated in a shaking incubator at the constant temperature of 4 ℃ for 12 h in a shaking manner, centrifuged and washed, and added into 1 mL of phosphate buffer solution with the pH = 7.38 to prepare a detection antibody hatching substance PtCuRNDFs-Ab2The solution was stored at 4 ℃ until use.
Example 8 detection of antibody hatching PtCu RNDFs-Ab2The solution was prepared by the following steps:
(1) preparation of PtCu RNDFs
Adding 0.28 g of hexadecyl trimethyl ammonium chloride into 35.0 mL of oleylamine, uniformly mixing, sequentially adding 0.03 g of platinum diacetylacetonate, 0.012 g of copper chloride dihydrate and 90 muL of diglycolamine, and carrying out ultrasonic treatment for 20 min; transferring to a stainless steel reaction kettle with a polytetrafluoroethylene lining, heating at 180 ℃ for reaction for 10 h, centrifugally cleaning the obtained product with an ethanol/cyclohexane 10:1 mixture for three times, and drying in vacuum at 60 ℃ to obtain PtCuRNDFs;
(2) detection of antibody hatchlings PtCu RNDFs-Ab2Preparation of the solution
2 mL of the PtCu RNDFs solution at a concentration of 2 mg/mL was added to 1 mL of the aflatoxin-detecting antibody solution Ab at a concentration of 10. mu.g/mL2In the step (b), the cells are incubated in a shaking incubator at the constant temperature of 4 ℃ for 12 h in a shaking manner, centrifuged and washed, and added into 2 mL of phosphate buffer solution with the pH = 7.38 to prepare a detection antibody hatching substance PtCuRNDFs-Ab2The solution was stored at 4 ℃ until use.
Example 9 detection of antibody hatching PtCu RNDFs-Ab2The solution was prepared by the following steps:
(1) preparation of PtCu RNDFs
Adding 0.30 g of hexadecyl trimethyl ammonium chloride into 40.0 mL of oleylamine, uniformly mixing, sequentially adding 0.04 g of platinum diacetyl acetone, 0.012 g of copper chloride dihydrate and 90 muL of diglycolamine, and carrying out ultrasonic treatment for 20 min; transferring to a stainless steel reaction kettle with a polytetrafluoroethylene lining, heating at 180 ℃ for 12 h, centrifugally cleaning the obtained product with an ethanol/cyclohexane 10:1 mixture for three times, and drying in vacuum at 60 ℃ to obtain PtCuRNDFs;
(2) detection of antibody hatchlings PtCu RNDFs-Ab2Preparation of the solution
3 mL of the PtCu RNDFs solution at a concentration of 2 mg/mL was added to 1.5 mL of the aflatoxin-detecting antibody solution Ab at a concentration of 10. mu.g/mL2In the step (b), the cells are incubated in a shaking incubator at the constant temperature of 4 ℃ for 12 h in a shaking manner, centrifuged and washed, and added into 3 mL of phosphate buffer solution with the pH = 7.38 to prepare a detection antibody hatching substance PtCuRNDFs-Ab2The solution was stored at 4 ℃ until use.
Example 10 detection of aflatoxin B1, the procedure was as follows:
(1) testing by using an electrochemical workstation in a three-electrode system, taking a saturated calomel electrode as a reference electrode, taking a platinum wire electrode as an auxiliary electrode, taking the prepared sensor as a working electrode, and testing in 10 mL of potassium ferricyanide solution containing 10 mmol/L;
(2) detecting aflatoxin B1 by a timed current method, selecting-0.4V as the detection of current measurement, wherein the input voltage is-0.4V, the sampling interval is 0.1 s, and the running time is 300 s;
(3) when the background current tends to be stable, 10 mu L of 5 mol/L hydrogen peroxide solution is injected into 10 mL of 50 mmol/L phosphate buffer solution with pH = 7.38 every 50 s, and the current change is recorded;
(4) and (3) determining the linear range of the aflatoxin B1 in the sample to be 10 pg/mL-60 ng/mL by adopting a standard curve method, wherein the detection limit is 3.33 pg/mL.
Example 11 detection of aflatoxin G1
The aflatoxin G1 in the sample is detected according to the method in the embodiment 10, the linear range is 10 pg-60 ng/mL, and the detection limit is 3.33 pg/mL.
Claims (4)
1. A preparation method of an electrochemical sensor based on PtCu RNDFs is characterized by comprising the following steps:
(1) al for glassy carbon electrode with diameter of 4 mm2O3Polishing the polishing powder into a mirror surface, and cleaning with ultrapure water;
(2) N-MoS of 6 muL and 1.0-3.0 mg/mL2Dripping QDs @ MWCNTs solution on the surface of the electrode, drying at room temperature, washing the surface of the electrode with ultrapure water, and drying;
(3) continuing to capture the aflatoxin capture antibody Ab of 6 muL and 8-12 mug/mL1Dropwise adding the solution to the surface of an electrode, washing with ultrapure water, and drying in a refrigerator at 4 ℃;
(4) continuously dropwise adding bovine serum albumin BSA solution with the mass fraction of 1% to the surface of the electrode by 3 muL, 0.5-1.5 mg/mL to seal non-specific active sites on the surface of the electrode, washing the surface of the electrode with ultrapure water, removing unbound BSA, and drying in a refrigerator at 4 ℃;
(5) continuously dropwise adding a series of aflatoxin antigen solutions with different concentrations, namely 6 muL and 10 pg/mL-60 ng/mL, washing the surface of the electrode with ultrapure water, and airing in a refrigerator at 4 ℃;
(6) continuously dropwise adding the detection antibody hatching substance PtCu RNDFs-Ab of 6 muL and 1.5-3.5 mg/mL2Incubating the solution on the surface of the electrode in a refrigerator at 4 deg.C for 40 min, washing with ultrapure water, and air dryingPreparing an electrochemical sensor based on PtCuRNDFs;
the PtCuRNDFs are all named as PtCu alloy dodecahedral nano frameworks;
the N-MoS2The preparation method of the QDs @ MWCNTs solution is characterized by comprising the following steps:
（1）N-MoS2preparation of QDs
Respectively weighing 0.2-0.7 g of molybdenum chloride and 1.0-3.0 g of thiourea, uniformly mixing, slowly adding 10 mL of ethanol, and stirring; after complete dissolution, continuously adding 2.0-4.0 g of nano silicon dioxide microspheres, carrying out ultrasonic treatment for 30 min, and drying at room temperature; then heating the mixture for 2-4 hours at 650 ℃ in a tubular furnace under the protection of argon; etching the obtained product with 30 mL of 5 mol/L sodium hydroxide for 24 h, and centrifugally cleaning the product for three times with ultrapure water to obtain the N-MoS2；
The N-MoS prepared above was added to 200 mL of N, N-dimethylformamide2 100 mg, ultrasonically treating in ice-water bath for 3 h, centrifuging at 3000 rpm for 10 min to obtain N-MoS2QDs；
（2）N-MoS2Preparation of QDs @ MWCNTs
Adding 10-30 mL of N-MoS into 25 mL and 1 mg/mL of carboxylated multi-walled carbon nano-tubes2QDs, stirring for 4 h after ultrasonic dispersion, centrifugally cleaning for three times by ultrapure water, and drying for 10 h in vacuum at 60 ℃ to obtain N-MoS2QDs@MWCNTs；
The detection antibody hatchery PtCu RNDFs-Ab2The preparation of the solution is characterized by comprising the following steps:
(1) preparation of PtCu RNDFs
Adding 0.25-0.30 g of hexadecyl trimethyl ammonium chloride into 30.0-40.0 mL of oleylamine, uniformly mixing, sequentially adding 0.02-0.04 g of platinum diacetylacetonate, 0.012 g of copper chloride dihydrate and 80-90 mu L of diglycolamine, and performing ultrasonic treatment for 20 min; transferring to a polytetrafluoroethylene-lined stainless steel reaction kettle, heating at 180 ℃ for reaction for 8-12 h, centrifugally cleaning the obtained product with an ethanol/cyclohexane 10:1 mixture for three times, and drying in vacuum at 60 ℃ to obtain PtCuRNDFs;
(2) detection of antibody hatchlings PtCu RNDFs-Ab2Preparation of the solution
Adding 1-3 mL of PtCu RNDFs solution with the concentration of 2 mg/mL into 0.5-1.5 mL of aflatoxin detection antibody solution Ab with the concentration of 10 mu g/mL2Performing shake incubation for 12 h in a constant temperature shaking box at 4 ℃, centrifuging and washing, adding into 1-3 mL of phosphoric acid buffer solution with pH = 7.38 to prepare the antibody hatching substance PtCuRNDFs-Ab for detection2The solution was stored at 4 ℃ until use.
2. The method for preparing the PtCu RNDFs-based electrochemical sensor according to claim 1, wherein the aflatoxin is selected from one of the following: aflatoxin B1, aflatoxin G1.
3. The PtCu RNDFs-based electrochemical sensor prepared by the preparation method according to claim 1, which is used for detecting aflatoxin, and is characterized in that the specific steps of the detection are as follows:
(1) testing by using an electrochemical workstation in a three-electrode system, taking a saturated calomel electrode as a reference electrode, taking a platinum wire electrode as an auxiliary electrode, taking the prepared sensor as a working electrode, and testing in 10 mL of potassium ferricyanide solution containing 10 mmol/L;
(2) detecting aflatoxin by a time-lapse current method, selecting-0.4V as the detection of current measurement, wherein the input voltage is-0.4V, the sampling interval is 0.1 s, and the running time is 300 s;
(3) when the background current tended to be stable, 10 μ L of 5 mol/L hydrogen peroxide solution was injected into 10 mL of 50 mmol/L phosphate buffer solution with pH = 7.38 every 50 s, and the change in current was recorded.
4. The electrochemical sensor of claim 3 for the detection of aflatoxins, wherein the aflatoxins are selected from one of the following: aflatoxin B1, aflatoxin G1.
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