CN106546649A - Au/MoS2Nano composite material glucose is without enzyme biologic sensor and preparation method thereof - Google Patents

Au/MoS2Nano composite material glucose is without enzyme biologic sensor and preparation method thereof Download PDF

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CN106546649A
CN106546649A CN201610910505.0A CN201610910505A CN106546649A CN 106546649 A CN106546649 A CN 106546649A CN 201610910505 A CN201610910505 A CN 201610910505A CN 106546649 A CN106546649 A CN 106546649A
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mos
composite material
nano composite
glucose
biologic sensor
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翟英娇
李金华
楚学影
徐铭泽
金芳军
方铉
魏志鹏
王晓华
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Changchun University of Science and Technology
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Changchun University of Science and Technology
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28—Electrolytic cell components
    • G01N27/30—Electrodes, e.g. test electrodes; Half-cells
    • G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
    • G01N27/3275—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction
    • G01N27/3277—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction being a redox reaction, e.g. detection by cyclic voltammetry

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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Apparatus Associated With Microorganisms And Enzymes (AREA)
  • Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)
  • Measurement Of The Respiration, Hearing Ability, Form, And Blood Characteristics Of Living Organisms (AREA)

Abstract

Au/MoS2Nano composite material glucose belongs to without enzyme biologic sensor technical field without enzyme biologic sensor and preparation method thereof.Prior art step is complicated, is difficult to grasp.The preparation method of the present invention is characterized in that, the flower-shaped MoS that will be prepared2Suspension pours the HAuCl of boiling into4In aqueous solution, Jing continues agitating heating makes Au Nanoparticle Modifieds to flower-shaped MoS2In, obtain Au/MoS2Nano composite material, finally by gained Au/MoS2Nano composite material is fixed on electrode and Au/MoS is obtained2Nano composite material glucose is without enzyme biologic sensor.The present invention without enzyme biologic sensor characterized in that, the Au/MoS2Nano composite material glucose is used to detect glucose concentration that detection method to be electrochemical process, and detection means is electrochemical workstation, by the Au/MoS without enzyme biologic sensor2Nano composite material glucose, as the working electrode in electrochemical workstation tested glucose solution is added in the electrolyte in electrochemical workstation without enzyme biologic sensor, judges the concentration of tested glucose solution according to Cyclic voltamogram curve.

Description

Au/MoS2Nano composite material glucose is without enzyme biologic sensor and preparation method thereof
Technical field
The present invention relates to a kind of Au/MoS2Nano composite material glucose is used without enzyme biologic sensor and preparation method thereof The flower-shaped MoS of Au Nanoparticle Modifieds of preparation2, obtain Au/MoS2Nano composite material, makes nothing using the nano composite material Enzyme biologic sensor, the Au/MoS of acquisition2Nano composite material can be used for quick detection blood glucose without enzyme biologic sensor Sugared concentration, belongs to without enzyme biologic sensor technical field.
Background technology
Prior art detects quickly and with sensitivity the concentration of glucose in blood using glucose enzyme sensor, to answer Diabetes harm to being on the rise.Enzyme electrode used by described glucose enzyme sensor is a kind of with platinum electrode as substrate Glucose oxidase electrode.
However, environmental factorss in the manufacturing process of sensor are easily received as biological sensitive materials using glucoseoxidase Affect and inactivate degeneration, such as the image of the factor such as temperature, humidity, pH value and surfactant；Meanwhile, glucoseoxidase is solid Method in the substrate is complicated and stability is poor, the stability of serious reduction enzyme sensor, repeatability.
There is a kind of Au/MoS in the prior art2Nano composite material without enzyme biologic sensor, the following institute of its preparation process State.
1st, by HAuCl4Rapidly join the NaBH of ice with sodium citrate dissolving in deionized water afterwards4, stir and be cooled to room Temperature, forms Au nanoparticles, preserves at a temperature of 4 DEG C；
2nd, by Na2MoO4Dissolving in deionized water, adjusts pH value to 6.5 with HCl, adds L-Cysteine stirring 1h, puts 48h is reacted at a temperature of 180 DEG C in entering reactor generate flower-shaped MoS2；
3rd, use HNO3/ deionized water, ethanol/deionized water pretreatment GCE (glass-carbon electrode)；
4th, cross-linking agent CS (Au- shitosans) is prepared using chemical method；
5th, by the flower-shaped MoS2The supersonic vibration in ethanol/deionized water forms uniform MoS2Suspension；
6th, the Au nanoparticles are mixed in proportion to form Au-CS mixed solutions with the cross-linking agent CS；
7th, with syringe first by the MoS2Hanging drop is coated on the GCE, is dried which with irradiation under infrared lamp, then Au-CS mixed solutions described in drop coating, natural air drying, form Au/MoS under crosslinked action thereon2Nanometer composite layer, system Into Au/MoS2Nano composite material is without enzyme biologic sensor.
However, methods described step is complicated, it is difficult to grasp；Two step drop coatings crosslinking film-forming process is wayward, may cause Fault of construction, reduces sensor performance.In addition, made is attempted detection bisphenol-A without enzyme biologic sensor.
The content of the invention
In order to obtain a kind of simple, controllable Au/MoS2Nano composite material is without enzyme biologic sensor preparation method, and obtains To a kind of Au/MoS for examination of glucose concentration2Nano composite material is without enzyme biologic sensor, it is proposed that a title For " Au/MoS2Nano composite material glucose is without enzyme biologic sensor and preparation method thereof " technical scheme.
A kind of Au/MoS2Nano composite material glucose is without enzyme biologic sensor preparation method, it is characterised in that will prepare Flower-shaped MoS2Suspension pours the HAuCl of boiling into4In aqueous solution, Jing continues agitating heating makes Au Nanoparticle Modifieds to flower-shaped MoS2In, obtain Au/MoS2Nano composite material, finally by gained Au/MoS2Nano composite material is fixed on electrode and Au/ is obtained MoS2Nano composite material glucose is without enzyme biologic sensor.
A kind of Au/MoS2Nano composite material glucose is without enzyme biologic sensor, it is characterised in that the Au/MoS2Nanometer Composite glucose is used to detect glucose concentration that detection method to be electrochemical process without enzyme biologic sensor, detection dress Electrochemical workstation is set to, by the Au/MoS2Nano composite material glucose is without enzyme biologic sensor as electrochemical operation Working electrode in standing, tested glucose solution is added in the electrolyte in electrochemical workstation, special according to cyclic voltammetric Linearity curve judges the concentration of tested glucose solution.
Its technique effect of the invention is as described below.
The method of the present invention is obtained Au/MoS in advance compared to prior art2Nano composite material, as shown in figure 1, no longer Realized by means of cross-linking agent this compound, then disposably biological sensitive materials are fixed in electrode basement using common process. Two-step reaction is successfully obtained Au/MoS2Nano composite material, step are simple, and technique is controllable.Using the method for the present invention, prepare Intermediate product MoS2Equally in flower-shaped, as shown in Figure 2 so that the biological sensitive materials for next preparing have bigger ratio table Area.Au Nanoparticle Modifieds are to flower-shaped MoS2Surface, as shown in Figure 3.Obtained Au/MoS2Nano composite material only contains Au, Mo, S element, it is very pure, as shown in Figure 4.
By the Au/MoS of the present invention2Nano composite material glucose is used to detect that glucose solution is dense without enzyme biologic sensor Degree, has preferable reversibility as working electrode, as shown in figure 5, Au nanoparticles have given play to preferable electronic conductivity, it is bright The aobvious Au/MoS improved as biological sensitive materials2The electronic conductivity of nano composite material so that Au/MoS2Nano combined material Electroactive site in expecting glucose without enzyme biologic sensor is increased, electric conductivity is improved, electron transmission ability strengthens, concrete manifestation Become easier in the electron transfer of working electrode surface, accelerate oxidation, the reduction process of tested glucose, sensing capabilities increase By force；This point is also verified by the Cyclic voltamogram curve obtained before and after actually detected glucose concentration, such as Fig. 6 institutes Show；Glucose concentration can accurately be detected in 0～30mM concentration ranges, as shown in fig. 7, sensitivity is higher；Tested There is more accurate linear relationship between the concentration and oxidation peak current value of glucose solution, as shown in figure 8, the explanation present invention Au/MoS2Nano composite material glucose is especially suitable for detecting glucose concentration without enzyme biologic sensor.
Compared with glucose enzyme sensor of the prior art, using the Au/MoS of the present invention2Nano composite material Fructus Vitis viniferae Sugar detects glucose concentration without enzyme biologic sensor, does not have the participation of glucoseoxidase, work electricity during the course of the reaction The glucose on pole surface is directly turned to gluconic acid by electrocatalytic oxidation, so as to improve its reaction rate, simple to operate, low cost, Stability is strong, reproducible.
Description of the drawings
Au/MoSs of the Fig. 1 for the present invention2Nano composite material glucose is without two in enzyme biologic sensor preparation method The flower-shaped MoS of two intermediate products that step is successively prepared2And Au/MoS2The XRD spectrum of nano composite material；In figure 2 θ= 14.13 °, 33.48 °, 39.73 °, 49.09 °, 59.07 ° of diffraction maximums for nearby occurring correspond respectively to 2H-MoS2(002), (101), (103), (105), (110) crystal face, with normal structure MoS2Diffraction maximum completely the same (JCPDS card 37-1492), Marked with square；The diffraction maximum occurred near 2 θ=38.184 °, 44.392 °, 64.576 ° in figure corresponds respectively to Au's (111), (200), (220) crystal face, (JCPDS card 04-0784) completely the same with normal structure Au diffraction maximums, use oval speckle Point mark.The method of the XRD spectrum explanation present invention is obtained Au/MoS through two steps2Nano composite material.
Fig. 2 is by the Au/MoS of the present invention2Nano composite material glucose is prepared without enzyme biologic sensor preparation method Au/MoS2The SEM photograph of nano composite material, shows prepared Au/MoS2It is in still flower-shaped (Au that nano composite material is overall The flower-shaped MoS of Nanoparticle Modified2MoS is not changed afterwards2Floriform appearance).
Fig. 3 is by the Au/MoS of the present invention2Nano composite material glucose is prepared without enzyme biologic sensor preparation method Au/MoS2The TEM photos of nano composite material, thus can be observed flower-shaped MoS2Piled up by several tiny " petals " on surface Form, " petal " is by stratiform MoS for bending again2Stacking is formed, and there are some nano-particle on " petal ", illustrates Au nanoparticles Son modification is in MoS2Surface.
Fig. 4 is by the Au/MoS of the present invention2Nano composite material glucose is prepared without enzyme biologic sensor preparation method Au/MoS2The EDS collection of illustrative plates of nano composite material, it is therefore seen that in Au/MoS2Only contain Mo, S, Au element in nano composite material, Illustrate that the intermediate product is very pure.
Au/MoSs of the Fig. 5 for the present invention2Cyclic voltamogram of the nano composite material glucose without enzyme biologic sensor is bent Line chart, the figure provide MoS simultaneously2The Cyclic voltamogram curve (NF is nickel foam) of/NF biosensors and NF bare electrodes.By This is visible, and three Cyclic voltamogram curves occur in that a pair stable, symmetrical redox peaks, illustrate that working electrode has Preferable reversibility；Compare MoS2/ NF, NF are identical to sweep Au/MoS under speed2/ NF has higher oxidoreduction peak current, this table Bright Au nanoparticles have preferable electronic conductivity, are modified in MoS2Biological sensitive materials have been effectively facilitated behind surface Electronic conductivity, so that the electron transfer of working electrode surface becomes easier to.
Fig. 6 is the Au/MoS using the present invention2Nano composite material glucose is molten without enzyme biologic sensor detection glucose The Cyclic voltamogram curve chart obtained before and after liquid concentration, the figure are given simultaneously and adopt MoS2Nano composite material glucose is without enzyme The Cyclic voltamogram curve chart obtained before and after biosensor detection glucose concentration, wherein curve a, c are respectively MoS2/NF、Au/MoS2(PBS solution is slow as the phosphate of electrolyte to the Cyclic voltamogram curves of/NF in PBS solution Rush solution), curve b, d are respectively MoS2/NF、Au/MoS2Circulations of/the NF after adding concentration to be 30mM glucoses in PBS solution VA characteristic curve.As can be seen here, when adding the glucose of same concentrations in the electrolytic solution, Au/MoS2The redox peaks of/NF Electric current is far above MoS2/ NF, and oxidation peak, to positive movement, to reverse movement, oxidoreduction peak current is significantly for reduction peak Increase, this is the Au/MoS due to the present invention2Nano composite material glucose without enzyme biologic sensor Fructus Vitis viniferae it is glycoxidative, reduction During effect it is obvious, increase its oxidation, reduction current, while Au/MoS2Nano composite material glucose is without the biological biography of enzyme Electroactive site in sensor is more, electric conductivity preferably, electron transmission ability it is stronger so that its glucose electrochemical sensing Can strengthen.
Fig. 7 is the Au/MoS using the present invention2Nano composite material glucose detects variable concentrations without enzyme biologic sensor One group of Cyclic voltamogram curve chart obtaining of glucose solution, the figure is simultaneously as Figure of abstract.It can be seen that correspondence There are a pair stable, symmetrical redox peaks in each concentration, with the increase redox peaks of glucose concentration Electric current gradually increases, and illustrates effective electron transfer is there occurs between glucose and working electrode.
Fig. 8 is the Au/MoS using the present invention2Nano composite material glucose is molten without enzyme biologic sensor detection glucose In liquid concentration, there is more accurate linear relationship, explanation between the concentration and oxidation peak current value of tested glucose solution The Au/MoS of the present invention2Nano composite material glucose is especially suitable for detecting glucose concentration without enzyme biologic sensor.
Specific embodiment
The Au/MoS of the present invention2Nano composite material glucose is without its specific embodiment of enzyme biologic sensor preparation method It is as described below.
1st, prepare flower-shaped MoS2Suspension.It is 7.3 × 10 by concentration-2The Na of M2MoO4It is 3.68 × 10 with concentration-1M's CH4N2S together, and concentration be 1.6 × 10-2The CTAB of M is successively poured in 50mL deionized waters, uniform stirring 15min, then PH value is adjusted to 8 with the NaOH that concentration is 2M, precursor solution is made；The precursor solution is heated to into 240 DEG C, is reacted 48h, is cooled to room temperature centrifuge dripping, does dried, in N after cleaning at a temperature of 60 DEG C2In 500 DEG C annealing 1h, obtain Obtain flower-shaped MoS2；By the flower-shaped MoS2The supersonic vibration in ethanol/deionized water forms unit for uniform suspension, and obtaining concentration is The flower-shaped MoS of 0.65mM2Suspension 10mL.
2nd, prepare Au/MoS2Nano composite material.By the 10mL flower-shaped MoS2Suspension pours the concentration of 50mL boilings into The HAuCl of 0.081mM4In aqueous solution, boiling a period of time again is persistently heated with stirring to, Au Nanoparticle Modifieds is made to flower-shaped MoS2In, stop heating, be cooled to centrifuge dripping after room temperature, dried done at a temperature of 40 DEG C after cleaning, obtain Au/MoS2Receive Nano composite material.
3rd, make Au/MoS2Nano composite material glucose is without enzyme biologic sensor.Method one：By the Au/MoS2Nanometer Composite and graphite powder, acetylene black, PVDF are according to 74:10:10:Mixed powder of 6 quality than mixing and stirring, to The mixed powder adds N-Methyl pyrrolidone to be tuned into slurry；The slurry is coated in NF substrates, at a temperature of 40 DEG C Dried is done, Au/MoS is obtained2Nano composite material glucose is without enzyme biologic sensor.Method two：By the Au/MoS2Nanometer Composite makes suspension, and the hanging drop is coated in GCE substrates, and dried is done in the irradiation under infrared lamp, obtains Au/ MoS2Nano composite material glucose is without enzyme biologic sensor.
The Au/MoS of the present invention2Nano composite material glucose is without the following institute of enzyme biologic sensor its specific embodiment State.
The Au/MoS2Nano composite material glucose is used to detect glucose concentration without enzyme biologic sensor.Inspection Survey method is electrochemical process, and detection means adopts the three-electrode electro Chemical work station of model CS350, by the Au/MoS2Receive Without enzyme biologic sensor as the working electrode in electrochemical workstation, Ag/AgCl is reference electrode to nano composite material glucose, Platinized platinum is to electrode (auxiliary electrode)；PBS solution (phosphate buffered solution) of the electrolyte for 0.1M concentration, wherein comprising 30mM The K of concentration3[Fe(CN)6] (potassium ferricyanide) and 30mM concentration K4Fe(CN)6(potassium ferrocyanide).By tested glucose solution It is added in the electrolyte in electrochemical workstation, the concentration of tested glucose solution is judged according to Cyclic voltamogram curve. The detectable concentration scope of tested glucose solution is 0～30mM.

Claims (7)

1. a kind of Au/MoS2Nano composite material glucose is without enzyme biologic sensor preparation method, it is characterised in that by what is prepared Flower-shaped MoS2Suspension pours the HAuCl of boiling into4In aqueous solution, Jing continues agitating heating makes Au Nanoparticle Modifieds to flower-shaped MoS2In, obtain Au/MoS2Nano composite material, finally by gained Au/MoS2Nano composite material is fixed on electrode and Au/ is obtained MoS2Nano composite material glucose is without enzyme biologic sensor.
2. Au/MoS according to claim 12, without enzyme biologic sensor preparation method, which is special for nano composite material glucose Levy and be, flower-shaped MoS2The preparation process of suspension is as described below, is 7.3 × 10 by concentration-2The Na of M2MoO4It is 3.68 with concentration ×10-1The CH of M4N2S together, and concentration be 1.6 × 10-2The CTAB of M is successively poured in 50mL deionized waters, uniform stirring 15min, then adjusts pH value to 8 with the NaOH that concentration is 2M, makes precursor solution；The precursor solution is heated to 240 DEG C, 48h is reacted, room temperature centrifuge dripping is cooled to, dried is done at a temperature of 60 DEG C after cleaning, in N2In 500 DEG C annealing 1h is processed, flower-shaped MoS is obtained2；By the flower-shaped MoS2The supersonic vibration in ethanol/deionized water forms unit for uniform suspension, obtains Flower-shaped MoS of the concentration for 0.65mM2Suspension.
3. Au/MoS according to claim 12, without enzyme biologic sensor preparation method, which is special for nano composite material glucose Levy and be, Au/MoS2The preparation process of nano composite material is as described below, by the flower-shaped MoS2Suspension pours 50mL boilings into Concentration for 0.081mM HAuCl4In aqueous solution, boiling a period of time again is persistently heated with stirring to, repaiies Au nanoparticles Adorn flower-shaped MoS2In, stop heating, be cooled to centrifuge dripping after room temperature, dried done at a temperature of 40 DEG C after cleaning, obtained Au/MoS2Nano composite material.
4. Au/MoS according to claim 12, without enzyme biologic sensor preparation method, which is special for nano composite material glucose Levy and be, Au/MoS2Manufacturing process of the nano composite material glucose without enzyme biologic sensor is as described below, method one：By institute State Au/MoS2Nano composite material and graphite powder, acetylene black, PVDF are according to 74:10:10:6 quality compares mixing and stirring Mixed powder, add N-Methyl pyrrolidone to be tuned into slurry to the mixed powder；The slurry is coated in NF substrates, Dried is done at a temperature of 40 DEG C, Au/MoS is obtained2Nano composite material glucose is without enzyme biologic sensor；Method two：By institute State Au/MoS2Nano composite material makes suspension, and the hanging drop is coated in GCE substrates, and the irradiation under infrared lamp does dry Dry process, obtains Au/MoS2Nano composite material glucose is without enzyme biologic sensor.
5. a kind of Au/MoS2Nano composite material glucose is without enzyme biologic sensor, it is characterised in that the Au/MoS2Nanometer is multiple Condensation material glucose is used to detect glucose concentration without enzyme biologic sensor, and detection method is electrochemical process, detection means For electrochemical workstation, by the Au/MoS2Nano composite material glucose is without enzyme biologic sensor as electrochemical workstation In working electrode, tested glucose solution is added in the electrolyte in electrochemical workstation, according to Cyclic voltamogram Curve judges the concentration of tested glucose solution.
6. Au/MoS according to claim 52Nano composite material glucose is without enzyme biologic sensor, it is characterised in that institute Three-electrode electro Chemical work station of the electrochemical workstation using model CS350 is stated, Ag/AgCl is reference electrode, and platinized platinum is right Electrode；PBS solution of the electrolyte for 0.1M concentration, wherein the K comprising 30mM concentration3[Fe(CN)6] and 30mM concentration K4Fe (CN)6。
7. Au/MoS according to claim 52Nano composite material glucose is without enzyme biologic sensor, it is characterised in that quilt The detectable concentration scope for surveying glucose solution is 0～30mM.
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CN107008458A (en) * 2017-05-10 2017-08-04 南昌航空大学 A kind of petal-shaped MoS2Load the preparation method of Au photochemical catalysts
CN108593733A (en) * 2018-03-17 2018-09-28 宁夏大学 Nanogold/molybdenum disulfide combination electrode and preparation method thereof and electrochemical sensor and its application
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CN109668951A (en) * 2018-11-27 2019-04-23 大连理工大学 One kind being based on MoS2Electrochemical sensing method of-AuNPs-PPY the composite material without enzyme detection glucose
CN109956500A (en) * 2019-03-25 2019-07-02 天津大学 A kind of preparation method of the molybdenum disulfide material of the nano flower-like for lithium sode cell cathode
CN110048095A (en) * 2019-03-25 2019-07-23 天津大学 A method of preparing the molybdenum disulfide molybdenum dioxide composite material for sodium ion negative electrode material
CN110346426A (en) * 2019-05-24 2019-10-18 陕西师范大学 Based on MoS2-The CPO biosensor and its detection NO of AuNPs and ionic liquid2-Application
CN110346426B (en) * 2019-05-24 2022-03-18 陕西师范大学 Based on MoS2CPO biosensor of AuNPs and ionic liquid and its detection of NO2-Application of
CN110470711A (en) * 2019-09-11 2019-11-19 江南大学 A kind of screen printing carbon electrode activation method
CN110470716A (en) * 2019-09-11 2019-11-19 江南大学 A kind of preparation method of the screen printing electrode of composite nano materials modification
CN110907249A (en) * 2019-12-13 2020-03-24 青岛农业大学 Glucose detection method based on composite nano enzyme system
CN110907249B (en) * 2019-12-13 2022-03-04 青岛农业大学 Glucose detection method based on composite nano enzyme system
CN111351828A (en) * 2020-04-11 2020-06-30 石河子大学 ZnFe2O4Preparation method and application of modified electrode material
CN112697765A (en) * 2020-11-11 2021-04-23 上海应用技术大学 Portable storage type surface enhanced Raman sensor, and preparation method, detection method and application thereof
CN112374540A (en) * 2020-11-27 2021-02-19 西北师范大学 Molybdenum disulfide composite zinc oxide gas-sensitive material with high response and recovery capacity and preparation process and application thereof
CN112892224A (en) * 2021-01-15 2021-06-04 东华大学 MoS2Preparation method and application of/CNT composite membrane
CN115060774A (en) * 2022-06-08 2022-09-16 华南理工大学 Preparation method and application of glycerol enzyme-free sensor
CN115591561A (en) * 2022-10-13 2023-01-13 福州大学（Cn） Nano-gold-doped molybdenum disulfide nanosheet with pyranose-like oxidase and horseradish peroxidase activities and application thereof
CN115591561B (en) * 2022-10-13 2024-03-29 福州大学 Nano gold doped molybdenum disulfide nanosheets with pyranose oxidase-like and horseradish peroxidase activities and application thereof

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