CN105758916A - Application and preparation method of deltamethrin photoelectrochemical sensor based on electrochemiluminescence excitation - Google Patents
Application and preparation method of deltamethrin photoelectrochemical sensor based on electrochemiluminescence excitation Download PDFInfo
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- CN105758916A CN105758916A CN201610148507.0A CN201610148507A CN105758916A CN 105758916 A CN105758916 A CN 105758916A CN 201610148507 A CN201610148507 A CN 201610148507A CN 105758916 A CN105758916 A CN 105758916A
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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
- G01N27/3278—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction involving nanosized elements, e.g. nanogaps or nanoparticles
Abstract
The invention discloses a preparation method of a functional nanomaterial based biological immunosensor with dual signal sending strategies of electrochemiluminescence and photoelectrochemistry.The sensor prepared according to the method has the advantages of simplicity in operation, portability, quickness in detection and low in cost and can be used for rapid and sensitive detection of deltamethrin in fields of daily production, daily life and the like.
Description
Technical field
The preparation method that the present invention relates to a kind of sensor for detecting decis, this sensor integration electrochemiluminescence and Optical Electro-Chemistry dual-use function.Belong to Nano-function thin films and electrochemical biosensor analysis technical field.
Background technology
Decis is the one that in chrysanthemum ester insecticide, virulence is the highest, to the toxic effect of insect up to 100 times of DDT, 40 times of parathion, have and tag and stomach poison function, action of contace poison is rapid, knock down power strong, not fumigating and systemic action, in higher concentrations some insects are had repellent action, the lasting period was up to 7～12 days.Decis belongs to poisoning poison class.Contact skin can cause irritation, red papules occurs；During acute poisoning, the lighter has headache, dizziness, Nausea and vomiting, inappetence, weak；Severe one it may also occur that fasciculation and tic.
At present, the method detecting decis mainly has chromatography, mass spectrography etc..This type of method instrument is valuable, complicated operation, and laboratory personnel just can detect after needing professional training.Therefore, R&D costs are low, it is fast, highly sensitive to detect, the decis sensor of high specificity is significant.
Electrochemical biosensor analytical technology, due to easy and simple to handle, the detection advantages such as speed is fast, obtains the attention of people day by day.The electrochemical biosensor analytical technology being presently used for detection decis is divided according to detection means and is mainly had electrochemical sensor, electrochemical luminous sensor and Optical Electro-Chemistry sensor three kinds.Wherein, electrochemical luminous sensor and Optical Electro-Chemistry sensor, relative to electrochemical sensor, have the features such as background signal noise is few, highly sensitive, testing cost is low, were paid close attention to by increasing researcher in recent years.
Electrochemiluminescence is also referred to as electrochemiluminescence, refer to and produce some special materials by electrochemical method at electrode surface, between these materials or and system in form excited state by electron transmission between other components, excited state return to ground state and produce luminescence phenomenon.Namely electrochemical luminous sensor by changing the decorative material of electrode surface, produces electrochemiluminescence with analyte, in optimal conditions, realizes the qualitative and quantitative analysis to analyte according to the associated change of analyte concentration with electrochemiluminescence intensity.
Optical Electro-Chemistry sensor is based on additional light source activation Electrophotosensitivmaterial material and causes that electron-hole pair is easily separated, under suitable inclined potential condition, it is achieved the electronics quick transmission on electrode, quasiconductor and trim and analyte, and forms photoelectric current.In optimal conditions, the change of analyte concentration can directly affect the size of photoelectric current, it is possible to realizes the qualitative and quantitative analysis to analyte according to the change of photoelectric current.
But, owing to electrochemical luminous sensor needs external optical signal to catch equipment such as photodiode etc., and Optical Electro-Chemistry sensor needs peripheral hardware light source to excite Electrophotosensitivmaterial material, this have impact on the convenience of the two operation to a certain extent, limits them and is more widely applied in actual production, life.Therefore, the electrochemical biosensor analytical technology designing, preparing more simple, fast detection decis has highly important practical value.
Summary of the invention
The preparation method that it is an object of the invention to provide a kind of simple to operate, easy to carry, detection is fast, cost is low decis sensor, prepared sensor, can be used for quick, the Sensitive Detection to decis in the fields such as daily production, life.Based on this purpose, the present invention, in same electrolyzer, adopts four electrode systems, namely two working electrodes, one to electrode and a reference electrode, wherein working electrode 1 adopts ITO electro-conductive glass, first modifies nickel phosphate ammonium micro-nano material NH herein above4NiPO4With gold nanorods Sol A uNRs as substrate, then electropolymerization luminol thereon, this electrode is as electrochemiluminescence working electrode W1, and working electrode 2 adopts titanium dioxide nanoplate colloidal sol TiO2NSs and decis antibody are modified jointly, as Optical Electro-Chemistry working electrode W2.When detecting, after adding fixed concentration hydrogen peroxide in electrolyzer, W1 applies step voltage, due to NH4NiPO4The effect of stabilized illumination and increase AuNRs load and NH4NiPO4With the concerted catalysis effect of AuNRs, luminol and hydroperoxidation, generation electrochemiluminescence, this is just equivalent to " turning on light ", and when step voltage is 0, electrochemiluminescence disappears, this is just equivalent to " turning off the light ", meanwhile applies constant voltage on W2, due to TiO always2NSs can because the luminescence that electrochemiluminescence produces excites causes that electron-hole pair is easily separated, it is marked at the horseradish peroxidase HRP catalyzing hydrogen peroxide generation oxygen that decis two resists, hydrogen peroxide is made to become hole " donor ", thus obtaining photoelectric current on W2, when electrogenerated chemiluminescence disappears, when namely " turning off the light ", photoelectric current disappears immediately.Due under the premise of fixing concentration of hydrogen peroxide, photoelectric current size and HRP concentration positive correlation, when in measured object, decis concentration is more big, when being attached on W2 with primary antibodie immunity, the concentration that immunity incorporation of markings has the decis two of HRP anti-again will be more big, the photoelectric current produced is also more big, the size of the photoelectric current of generation and decis concentration positive correlation, therefore can realize the detection to decis by the size of recording light electric current.
Based on above inventive principle, the concrete technical scheme that the present invention adopts is as follows:
1. a preparation method for the decis Optical Electro-Chemistry sensor excited based on electrochemiluminescence, it is characterized in that, preparation process is:
(1) preparation method of electrochemiluminescence working electrode W1, described W1 is by NH4NiPO4With prepare after electropolymerization luminol on the AuNRs ITO electro-conductive glass jointly modified, be characterized in, concrete preparation process is:
1) with ITO electro-conductive glass for working electrode, at electrode surface drop coating NH4NiPO4Solution, area coverage is 1cm × 1cm, dries under room temperature；
2) by 1) working electrode that obtains, at NH4NiPO4Surface drop coating AuNRs, area coverage is 1cm × 1cm, dries under room temperature；
3) by 2) working electrode that obtains, immerse in electrolyte, immersion area is NH4NiPO4The area common covered with AuNRs, utilizes three-electrode system that working electrode is carried out electrochemical deposition, takes out working electrode after deposition, uses ultra-pure water to clean, and at 4 DEG C, lucifuge dries, and prepares electrochemiluminescence working electrode W1；
Described NH4NiPO4Solution is nickel phosphate ammonium micro-nano material aqueous solution, and described nickel phosphate ammonium micro-nano material is porous flake micro-nano material, described NH4NiPO4Preparation process be: in 40mL water, add 2.0 ~ 4.0g ammonium salt and 0.15 ~ 0.25g phosphate, after being completely dissolved, add 0.15 ~ 0.25g Nickel Chloride, at 30 ~ 45 DEG C, stir 10 ~ 14h, centrifugation, product is placed at 50 DEG C dry, namely obtains NH4NiPO4；
Described ammonium salt is selected from one of following: ammonium chloride, ammonium bromide, ammonium phosphate, ammonium dihydrogen phosphate, diammonium phosphate；
Described phosphate is selected from one of following: ammonium phosphate, ammonium dihydrogen phosphate, diammonium phosphate；
Described AuNRs is the aqueous solution of gold nanorods, and described gold nanorods is bar-like golden nanometer particle, and length is 20 ~ 40nm；
Described electrolyte is the sulfuric acid solution containing luminol, and in described electrolyte, the concentration of luminol is 1 ~ 10mmol/L, and sulfuric acid concentration is 0.1 ~ 1.0mol/L；
Described three-electrode system, including working electrode, reference electrode and to electrode, described reference electrode is saturated calomel electrode, and described is platinum electrode to electrode；
Described electrochemical deposition process, the electrochemical method of employing is cyclic voltammetry, and starting voltage is-0.2V, and final voltage is 1.5V, sweeps speed for 100mv/s, circulation 20 ~ 30 circle；
(2) preparation method of Optical Electro-Chemistry working electrode W2, described W2 is by TiO2The ITO electro-conductive glass that NSs and decis antibody are modified jointly, is characterized in, concrete preparation process is:
1) with ITO electro-conductive glass for working electrode, at electrode surface drop coating 8 ~ 12 μ LTiO2NSs, dries under room temperature；
2) by 1) in the working electrode that obtains put in Muffle furnace, be annealed processing at 450 DEG C, after process, be cooled to room temperature；
3) by 2) in working electrode surface drop coating 8 ~ 12 μ L decis antibody that obtains, dry at 4 DEG C, clean with ultra-pure water after drying, dry at 4 DEG C, prepare Optical Electro-Chemistry working electrode W2；
Described TiO2NSs is the aqueous solution of the titanium dioxide nanoplate of 1mg/mL, and described titanium dioxide nanoplate is the titanium dioxide nano-particle of square lamellar, and the length of side is 60 ~ 80nm；
The concentration of described decis antibody-solutions is 300 μ g/mL；
(3) preparation method of the decis Optical Electro-Chemistry sensor excited based on electrochemiluminescence:
1) one side that W1 and W2 conducts electricity relatively being inserted in electrolyzer, W1 and W2 spacing is 0.5cm ~ 1.5cm；
2) with Ag/AgCl be reference electrode RE, platinum electrode be to electrode CE, insert in electrolyzer, collectively constitute four electrode systems with W1 and W2；
3) in electrolyzer add 10mLpH value be 11 ~ 13 NaOH solution and 0.2mL concentration be the hydrogenperoxide steam generator of 1mmol/L；
4) by 1) ~ 3) obtained by four electrode systems and electrolyzer be placed in magazine, namely prepare the decis Optical Electro-Chemistry sensor excited based on electrochemiluminescence.
2. the detection being applied to hydrogen peroxide of decis Optical Electro-Chemistry sensor of the present invention, the detection method being characterized in concrete is:
(1) on W2, drip the decis standard solution of 10 μ L variable concentrations, after hatching 30min, decis and the decis antibody on W2 carry out immunity combination, after flushing, the decis two dripping 10 μ L horseradish peroxidase HRP labellings again resists, and after hatching 30min, the decis two of HRP labelling is anti-carries out immunity combination with decis, after flushing, prepare W2 to be measured；
(2) utilizing electrochemical workstation, adopt the method for step voltage that W1 applies step voltage on W1, initial voltage is 0v, and step voltage is 0.7 ~ 0.9v, and snap time is 10 ~ 30s；Meanwhile, when adopting on W2 to be measured, W2 to be measured is applied constant voltage by m-current methods, and voltage is 0 ~ 0.6v；Electric current on W2 to be measured can increase accordingly along with the increase of decis concentration, according to the relation between gained electric current increase value and decis concentration, drawing curve；；
(3) decis solution to be measured replaces the standard solution of decis, and the decis detection method described in (1) and (2) detects, and draws the concentration of decis solution to be measured according to obtained electric current increase value and the working curve drawn；
The concentration that the decis two of described HRP labelling is anti-is 300 μ g/mL.
The useful achievement of the present invention
(1) decis Optical Electro-Chemistry sensor of the present invention preparation is simple, easy to operate, it is not necessary to external accessory, utilize the microminiaturization of detection equipment, portability, and achieve the selective enumeration method quick, sensitive, high to hydrogen peroxide, there is wide market development prospect；
(2) present invention adopts four electrode system detection decises first in same electrolyzer, and achieves electrogenerated chemiluminescence signal amplification strategy difunctional with Optical Electro-Chemistry.Along with the increase of decis concentration in electrolyzer, the decis two of the HRP labelling being modified on W2 is anti-will be increased, and also implies that HRP is to hydrogen peroxide catalyzed raising.Since so, on the one hand, make electrogenerated chemiluminescence intensity linearly increasing, the linear increase of photoelectric current excited；On the other hand, hydrogen peroxide is as electron donor so that the linear increase of photoelectric current in Optical Electro-Chemistry reaction.Therefore, electrogenerated chemiluminescence and two kinds of methods of Optical Electro-Chemistry are reaction jointly, interaction in same electrolyzer, under same electrochemical workstation, achieve the dual amplification that decis is detected the signal of telecommunication, drastically increase detection sensitivity and detection limit, there is important scientific meaning and using value.
Detailed description of the invention
Embodiment 1A kind of decis Optical Electro-Chemistry sensor excited based on electrochemiluminescence, concrete preparation process is:
(1) preparation of electrochemiluminescence working electrode W1:
1) with ITO electro-conductive glass for working electrode, at electrode surface drop coating NH4NiPO4Solution, area coverage is 1cm × 1cm, dries under room temperature；
2) by 1) working electrode that obtains, at NH4NiPO4Surface drop coating AuNRs, area coverage is 1cm × 1cm, dries under room temperature；
3) by 2) working electrode that obtains, immerse in electrolyte, immersion area is NH4NiPO4The area common covered with AuNRs, utilizes three-electrode system that working electrode is carried out electrochemical deposition, takes out working electrode after deposition, uses ultra-pure water to clean, and at 4 DEG C, lucifuge dries, and prepares electrochemiluminescence working electrode W1；
Described NH4NiPO4Solution is nickel phosphate ammonium micro-nano material aqueous solution, the preparation process of described nickel phosphate ammonium micro-nano material is: add 2.0 ~ 4.0g ammonium salt and 0.15 ~ 0.25g phosphate in 40mL water, after being completely dissolved, add 0.15 ~ 0.25g Nickel Chloride, 10 ~ 14h is stirred at 30 ~ 45 DEG C, centrifugation, is placed in product at 50 DEG C dry, namely obtains NH4NiPO4；
Described ammonium salt is selected from one of following: ammonium chloride, ammonium bromide, ammonium phosphate, ammonium dihydrogen phosphate, diammonium phosphate；
Described phosphate is selected from one of following: ammonium phosphate, ammonium dihydrogen phosphate, diammonium phosphate；
Described AuNRs is the aqueous solution of gold nanorods, and described gold nanorods is bar-like golden nanometer particle, and length is 20nm；
Described electrolyte is the sulfuric acid solution containing luminol, and in described electrolyte, the concentration of luminol is 1mmol/L, and sulfuric acid concentration is 0.1mol/L；
Described three-electrode system, including working electrode, reference electrode and to electrode, described reference electrode is saturated calomel electrode, and described is platinum electrode to electrode；
Described electrochemical deposition process, the electrochemical method of employing is cyclic voltammetry, and starting voltage is-0.2V, and final voltage is 1.5V, sweeps speed for 100mv/s, circulation 20 ~ 30 circle.
(2) preparation of Optical Electro-Chemistry working electrode W2:
1) with ITO electro-conductive glass for working electrode, at electrode surface drop coating 8 μ LTiO2NSs, dries under room temperature；
2) by 1) in the working electrode that obtains put in Muffle furnace, be annealed processing at 450 DEG C, after process, be cooled to room temperature；
3) by 2) in the working electrode surface drop coating 8 μ L decis antibody-solutions that obtains, dry at 4 DEG C, clean with ultra-pure water after drying, dry at 4 DEG C, prepare Optical Electro-Chemistry working electrode W2；
Described TiO2NSs is the aqueous solution of the titanium dioxide nanoplate of 1mg/mL, and described titanium dioxide nanoplate is the titanium dioxide nano-particle of square lamellar, and the length of side is 60 ~ 80nm；
The concentration of described decis antibody-solutions is 300 μ g/mL；
(3) preparation method of the decis Optical Electro-Chemistry sensor excited based on electrochemiluminescence:
1) being inserted face to face in electrolyzer by the W1 of preparation in (1) and the W2 of (2) middle preparation, W1 and W2 spacing is 0.5cm；
2) with Ag/AgCl be reference electrode RE, platinum electrode be to electrode CE, insert in electrolyzer, collectively constitute four electrode systems with W1 and W2；
3) in electrolyzer add 10mLpH value be 11 NaOH solution and 0.2mL concentration be the hydrogenperoxide steam generator of 1mmol/L；
4) by 1) ~ 3) obtained by four electrode systems and electrolyzer be placed in magazine, namely prepare the decis Optical Electro-Chemistry sensor excited based on electrochemiluminescence.
Embodiment 2A kind of decis Optical Electro-Chemistry sensor excited based on electrochemiluminescence, concrete preparation process is:
(1) preparation of electrochemiluminescence working electrode W1:
Preparation process is with the preparation process of W1 in embodiment 1, difference is: in the preparation process of nickel phosphate ammonium micro-nano material, ammonium salt addition is 0.3g, phosphate addition is 0.20g, and Nickel Chloride addition is 0.20g, whipping temp and time respectively 38 DEG C and 12h；The length of gold nanorods is 30nm；In electrolyte, the concentration of luminol is 5mmol/L, and sulfuric acid concentration is 0.5mol/L；When cyclic voltammetry carries out electrochemical deposition, circulation 25 circle.
(2) preparation of Optical Electro-Chemistry working electrode W2:
1) with ITO electro-conductive glass for working electrode, at electrode surface drop coating 10 μ LTiO2NSs, dries under room temperature；
2) by 1) in the working electrode that obtains put in Muffle furnace, be annealed processing at 450 DEG C, after process, be cooled to room temperature；
3) by 2) in the working electrode surface drop coating 10 μ L decis antibody-solutions that obtains, dry at 4 DEG C, clean with ultra-pure water after drying, dry at 4 DEG C, prepare Optical Electro-Chemistry working electrode W2；
All the other are with the preparation process of W2 in embodiment 1.
(3) preparation method of the decis Optical Electro-Chemistry sensor excited based on electrochemiluminescence:
Preparation process is with embodiment 1, and difference is W1 and W2 spacing is 1.0cm, and the pH value of the NaOH solution added in electrolyzer is 12.
Embodiment 3A kind of decis Optical Electro-Chemistry sensor excited based on electrochemiluminescence, concrete preparation process is:
(1) preparation of electrogenerated chemiluminescence working electrode W1:
Preparation process is with the preparation process of W1 in embodiment 1, difference is: in the preparation process of nickel phosphate ammonium micro-nano material, ammonium salt addition is 0.4g, phosphate addition is 0.25g, and Nickel Chloride addition is 0.25g, whipping temp and time respectively 45 DEG C and 14h；The length of gold nanorods is 40nm；In electrolyte, the concentration of luminol is 10mmol/L, and sulfuric acid concentration is 1.0mol/L；When cyclic voltammetry carries out electrochemical deposition, circulation 30 circle.
(2) preparation of Optical Electro-Chemistry working electrode W2:
1) with ITO electro-conductive glass for working electrode, at electrode surface drop coating 12 μ LTiO2NSs, dries under room temperature；
2) by 1) in the working electrode that obtains put in Muffle furnace, be annealed processing at 450 DEG C, after process, be cooled to room temperature；
3) by 2) in the working electrode surface drop coating 12 μ L decis antibody-solutions that obtains, dry at 4 DEG C, clean with ultra-pure water after drying, dry at 4 DEG C, prepare Optical Electro-Chemistry working electrode W2；
All the other are with the preparation process of W2 in embodiment 1.
(3) preparation method of the decis Optical Electro-Chemistry sensor excited based on electrochemiluminescence:
Preparation process is with embodiment 1, and difference is W1 and W2 spacing is 1.5cm, and the pH value of the NaOH solution added in electrolyzer is 13.
Embodiment 4A kind of application of the decis Optical Electro-Chemistry sensor excited based on electrochemiluminescence
A kind of decis Optical Electro-Chemistry sensor excited based on electrochemiluminescence of embodiment 1 preparation is applied to the detection of decis, and its detecting step is:
(1) on W2, drip the decis standard solution of 10 μ L variable concentrations, after hatching 30min, decis and the decis antibody on W2 carry out immunity combination, after flushing, the decis two dripping 10 μ L horseradish peroxidase HRP labellings again resists, and after hatching 30min, the decis two of HRP labelling is anti-carries out immunity combination with decis, after flushing, prepare W2 to be measured；
(2) utilizing electrochemical workstation, adopt the method for step voltage that W1 applies step voltage on W1, initial voltage is 0v, and step voltage is 0.7v, and snap time is 10s；Meanwhile, when adopting on W2 to be measured, W2 to be measured is applied constant voltage by m-current methods, and voltage is 0v；Electric current on W2 to be measured can increase accordingly along with the increase of decis concentration, according to the relation between gained electric current increase value and decis concentration, drawing curve；
(3) decis solution to be measured replaces the standard solution of decis, and the decis detection method described in (1) and (2) detects, and draws the concentration of decis solution to be measured according to obtained electric current increase value and the working curve drawn；
The concentration that the decis two of described HRP labelling is anti-is 300 μ g/mL.
Embodiment 5A kind of application of the decis Optical Electro-Chemistry sensor excited based on electrochemiluminescence
A kind of decis Optical Electro-Chemistry sensor excited based on electrochemiluminescence of embodiment 2 preparation is applied to the detection of decis, and its detecting step is except following steps, and all the other steps are with embodiment 4:
Step (2) utilizes electrochemical workstation, adopts the method for step voltage that W1 applies step voltage on W1, and initial voltage is 0v, and step voltage is 0.8v, and snap time is 20s；Meanwhile, when adopting on W2 to be measured, W2 to be measured is applied constant voltage by m-current methods, and voltage is 0.3v；Electric current on W2 to be measured can increase accordingly along with the increase of decis concentration, according to the relation between gained electric current increase value and decis concentration, drawing curve.
Embodiment 6A kind of application of the decis Optical Electro-Chemistry sensor excited based on electrochemiluminescence
A kind of decis Optical Electro-Chemistry sensor excited based on electrochemiluminescence of embodiment 3 preparation is applied to the detection of decis, and its detecting step is except following steps, and all the other steps are with embodiment 4:
Step (2) utilizes electrochemical workstation, adopts the method for step voltage that W1 applies step voltage on W1, and initial voltage is 0v, and step voltage is 0.9v, and snap time is 30s；Meanwhile, when adopting on W2 to be measured, W2 to be measured is applied constant voltage by m-current methods, and voltage is 0.6v；Electric current on W2 to be measured can increase accordingly along with the increase of decis concentration, according to the relation between gained electric current increase value and decis concentration, drawing curve.
Embodiment 7Decis Optical Electro-Chemistry sensor prepared by embodiment 1-3, is applied to the detection of decis according to the detecting step of embodiment 4-6, has excellent Detection results, and detection is limited to 20pmol/L.
Claims (6)
1. the preparation method of the decis Optical Electro-Chemistry sensor excited based on electrochemiluminescence, it is characterised in that adopt nickel phosphate ammonium micro-nano material NH4NiPO4With after electropolymerization luminol on the gold nanorods Sol A uNRs ITO electro-conductive glass jointly modified as electrochemiluminescence working electrode W1, titanium dioxide nanoplate colloidal sol TiO2The ITO electro-conductive glass that NSs and decis antibody are modified jointly is as Optical Electro-Chemistry working electrode W2, Ag/AgCl electrode as reference electrode RE, platinum electrode as to electrode CE, four electrodes are inserted jointly same electrolyzer forms four electrode systems, four prepared electrode systems are placed in magazine, namely prepare the decis Optical Electro-Chemistry sensor excited based on electrochemiluminescence.
2. the preparation method of the decis Optical Electro-Chemistry sensor excited based on electrochemiluminescence according to claim 1, it is characterised in that described nickel phosphate ammonium micro-nano material NH4NiPO4For porous flake micro-nano material.
3. the preparation method of the decis Optical Electro-Chemistry sensor excited based on electrochemiluminescence according to claim 1, it is characterized in that, the described aqueous solution that gold nanorods Sol A uNRs is gold nanorods, described gold nanorods is bar-like golden nanometer particle, and length is 20 ~ 40nm.
4. the preparation method of the decis Optical Electro-Chemistry sensor excited based on electrochemiluminescence according to claim 1, it is characterised in that described titanium dioxide nanoplate colloidal sol TiO2NSs is the aqueous solution of titanium dioxide nanoplate, and described titanium dioxide nanoplate is the titanium dioxide nano-particle of square lamellar, and the length of side is 60 ~ 80nm.
5. the preparation method of the decis Optical Electro-Chemistry sensor excited based on electrochemiluminescence according to claim 1, it is characterised in that the one side that W1 and W2 conducts electricity relatively being inserted in electrolyzer, W1 and W2 spacing is 0.5cm ~ 1.5cm.
6. the decis Optical Electro-Chemistry sensor that prepared by preparation method according to claim 1, it is characterised in that described decis Optical Electro-Chemistry sensor is applied to the detection of decis, and detecting step is:
(1) on W2, decis solution to be measured is dripped, after the decis in decis solution to be measured decis antibody mediated immunity on W2 is combined, rinse out all the other materials, drip that the decis two of horseradish peroxidase HRP labelling is anti-carries out immunity combination again, the decis two washing unnecessary HRP labelling in conjunction with backlash off resists, and prepares W2 to be measured；
(2) utilizing electrochemical workstation, in the electrolyte containing fixed concentration hydrogen peroxide, adopt the method for step voltage that W1 applies step voltage on W1, initial voltage is 0v, and step voltage is 0.7 ~ 0.9v, and snap time is 10 ~ 30s；Meanwhile, when adopting on W2 to be measured, W2 to be measured is applied constant voltage by m-current methods, and voltage is 0 ~ 0.6v；Electric current on W2 to be measured can along with in decis solution to be measured the concentration of decis increase and increase accordingly, increasing according to gained electric current is worth in decis solution to be measured the concentration of decis.
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| CN110579612A (en) * | 2019-10-17 | 2019-12-17 | 桂林理工大学 | Surface plasma resonance immunoassay method for embedded Au nano-film electrode |
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