CN105806832A - Preparation method and application of hydrogen peroxide sensor based on double functions of electrochemiluminescence and photoelectrochemistry - Google Patents
Preparation method and application of hydrogen peroxide sensor based on double functions of electrochemiluminescence and photoelectrochemistry Download PDFInfo
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Abstract
The invention discloses a preparation method of hydrogen peroxide sensor which has electrochemiluminescence and photoelectrochemistry double functions and is constructed on the basis of a functional nano material.The prepared sensor is easy to operate, convenient to carry, rapid in inspection, low in cost and capable of being used for rapid and sensitive detection on hydrogen peroxide in the fields of daily production and life and the like.
Description
Technical field
The preparation method that the present invention relates to a kind of sensor for detecting hydrogen peroxide, this sensor integration electrogenerated chemiluminescence and Optical Electro-Chemistry dual-use function.Belong to Nano-function thin films and electrochemical biosensor analysis technical field.
Background technology
Hydrogen peroxide is a kind of oxidant, generally can be decomposed into water and oxygen, but it is slow, when adding catalyst (or enzyme), response speed is accelerated, thus can be made instantly available the amount of hydrogen peroxide or the amount of catalyst (or enzyme), hydrogen peroxide also often exists with the form of reaction intermediate in vivo simultaneously, therefore, hydrogen peroxide all plays important role in fields such as medical diagnosis, clinical treatment, environment measuring and food productions, and research and development hydrogen peroxide detection method also just has highly important using value.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 hydrogen peroxide is divided according to detection means and is mainly had electrochemical sensor, Electrochemiluminescsensor sensor and Optical Electro-Chemistry sensor three kinds.Wherein, Electrochemiluminescsensor 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.
Electrogenerated chemiluminescence 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 Electrochemiluminescsensor 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 Electrochemiluminescsensor 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 hydrogen peroxide 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 hydrogen peroxide sensor, prepared sensor, can be used for quick, the Sensitive Detection to hydrogen peroxide in the fields such as daily production, life.Based on this purpose, the present invention is in same electrolyzer, adopt four electrode systems, namely two working electrodes, one to electrode and a reference electrode, wherein working electrode 1 adopts gold palladium nanometer rods Sol A uPdNRs and electropolymerization luminol jointly to modify, as electrogenerated chemiluminescence working electrode W1, working electrode 2 adopts titanium dioxide nanoplate colloidal sol TiO2NSs and horseradish peroxidase Solution H RP modifies jointly, as Optical Electro-Chemistry working electrode W2.When detecting, after electrolyzer adds hydrogen peroxide, W1 applies step voltage, due to the catalytic action of AuPdNRs, luminol and hydroperoxidation, producing electrogenerated chemiluminescence, this is just equivalent to " turning on light ", when step voltage is 0, electrogenerated chemiluminescence 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 electrogenerated chemiluminescence produces excites causes that electron-hole pair is easily separated, HRP catalyzing hydrogen peroxide produces oxygen, 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, the size of the photoelectric current produced and concentration of hydrogen peroxide positive correlation, therefore can realize the detection to hydrogen peroxide 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. based on a preparation method for the bifunctional hydrogen peroxide sensor of electrogenerated chemiluminescence and Optical Electro-Chemistry, it is characterized in that, preparation process is:
(1) preparation method of electrogenerated chemiluminescence working electrode W1, described W1 is the ITO electro-conductive glass jointly modified by AuPdNRs and electropolymerization luminol, is characterized in, concrete preparation process is:
1) with ITO electro-conductive glass for working electrode, at electrode surface drop coating AuPdNRs, area coverage is 1cm × 1cm, dries under room temperature；
2) by 1) working electrode that obtains, immerse in electrolyte, immersing area is the AuPdNRs area covered, utilize three-electrode system that working electrode is carried out electrochemical deposition, after deposition, take out working electrode, use ultra-pure water to clean, at 4 DEG C, lucifuge dries, and prepares electrogenerated chemiluminescence working electrode W1；
Described AuPdNRs is the aqueous solution of the rod-like nano material of nucleocapsid structure, the rod-like nano material of described nucleocapsid structure is with gold nanorods for core, Pd nano particle is the rod-like nano material of shell, 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 HRP modifies 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 LHRP 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；
Described HRP is the horseradish peroxidase aqueous solution of 5mU/mL；
(3) based on the preparation method of the bifunctional hydrogen peroxide sensor of electrogenerated chemiluminescence and Optical Electro-Chemistry:
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) adding 10mLpH value in electrolyzer is the NaOH solution of 11 ~ 13；
4) by 1) ~ 3) obtained by four electrode systems and electrolyzer be placed in magazine, namely prepare based on the bifunctional hydrogen peroxide sensor of electrogenerated chemiluminescence and Optical Electro-Chemistry.
2. the detection being applied to hydrogen peroxide of hydrogen peroxide sensor of the present invention, the detection method being characterized in concrete is:
(1) 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, W2 is applied constant voltage by m-current methods, and voltage is 0 ~ 0.6v；
(2) adding the Hydrogen peroxide standard solution of variable concentrations in electrolyzer, the electric current on W2 can increase accordingly along with the increase of concentration of hydrogen peroxide, according to the relation between gained electric current increase value and concentration of hydrogen peroxide, drawing curve；
(3) hydrogenperoxide steam generator to be measured replaces the standard solution of hydrogen peroxide, and the hydrogen peroxide detection method described in (1) and (2) detects, and draws the concentration of hydrogenperoxide steam generator to be measured according to obtained electric current increase value and the working curve drawn.
The useful achievement of the present invention
(1) hydrogen peroxide 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 hydrogen peroxide first in same electrolyzer, and achieves electrogenerated chemiluminescence signal amplification strategy difunctional with Optical Electro-Chemistry.Along with the increase of concentration of hydrogen peroxide in electrolyzer, 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 hydrogen peroxide 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 based on the bifunctional hydrogen peroxide sensor of electrogenerated chemiluminescence and Optical Electro-Chemistry, concrete preparation process is:
(1) preparation of electrogenerated chemiluminescence working electrode W1:
1) with ITO electro-conductive glass for working electrode, at electrode surface drop coating AuPdNRs, area coverage is 1cm × 1cm, dries under room temperature；
2) by 1) working electrode that obtains, immerse in electrolyte, immersing area is the AuPdNRs area covered, utilize three-electrode system that working electrode is carried out electrochemical deposition, after deposition, take out working electrode, use ultra-pure water to clean, at 4 DEG C, lucifuge dries, and prepares electrogenerated chemiluminescence working electrode W1；
Described AuPdNRs is the aqueous solution of the rod-like nano material of nucleocapsid structure, and the rod-like nano material of described nucleocapsid structure is with gold nanorods for core, and Pd nano particle is the rod-like nano material of shell, 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 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 LHRP 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；
Described HRP is the horseradish peroxidase aqueous solution of 5mU/mL.
(3) based on the preparation method of the bifunctional hydrogen peroxide sensor of electrogenerated chemiluminescence and Optical Electro-Chemistry:
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) adding 10mLpH value in electrolyzer is the NaOH solution of 11；
4) by 1) ~ 3) obtained by four electrode systems and electrolyzer be placed in magazine, namely prepare based on the bifunctional hydrogen peroxide sensor of electrogenerated chemiluminescence and Optical Electro-Chemistry.
Embodiment 2A kind of based on the bifunctional hydrogen peroxide sensor of electrogenerated chemiluminescence and Optical Electro-Chemistry, concrete preparation process is:
(1) preparation of electrogenerated chemiluminescence working electrode W1:
Preparation process is with the preparation process of W1 in embodiment 1, and the length that difference is gold nanorods is 30nm, and in electrolyte, the concentration of luminol is 5mmol/L, and sulfuric acid concentration is 0.5mol/L, when cyclic voltammetry carries out electrochemical deposition, and 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 LHRP 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) based on the preparation method of the bifunctional hydrogen peroxide sensor of electrogenerated chemiluminescence and Optical Electro-Chemistry:
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 based on the bifunctional hydrogen peroxide sensor of electrogenerated chemiluminescence and Optical Electro-Chemistry, concrete preparation process is:
(1) preparation of electrogenerated chemiluminescence working electrode W1:
Preparation process is with the preparation process of W1 in embodiment 1, and the length that difference is gold nanorods is 40nm, and in electrolyte, the concentration of luminol is 10mmol/L, and sulfuric acid concentration is 1.0mol/L, when cyclic voltammetry carries out electrochemical deposition, and 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 LHRP 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) based on the preparation method of the bifunctional hydrogen peroxide sensor of electrogenerated chemiluminescence and Optical Electro-Chemistry:
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 based on the bifunctional hydrogen peroxide sensor of electrogenerated chemiluminescence and Optical Electro-Chemistry
A kind of detection being applied to hydrogen peroxide based on the bifunctional hydrogen peroxide sensor of electrogenerated chemiluminescence and Optical Electro-Chemistry of embodiment 1 preparation, its detecting step is:
(1) 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, W2 is applied constant voltage by m-current methods, and voltage is 0v；
(2) adding the Hydrogen peroxide standard solution of variable concentrations in electrolyzer, the electric current on W2 can increase accordingly along with the increase of concentration of hydrogen peroxide, according to the relation between gained electric current increase value and concentration of hydrogen peroxide, drawing curve；
(3) hydrogenperoxide steam generator to be measured replaces the standard solution of hydrogen peroxide, and the hydrogen peroxide detection method described in (1) and (2) detects, and draws the concentration of hydrogenperoxide steam generator to be measured according to obtained electric current increase value and the working curve drawn.
Embodiment 5A kind of application based on the bifunctional hydrogen peroxide sensor of electrogenerated chemiluminescence and Optical Electro-Chemistry
A kind of detection being applied to hydrogen peroxide based on the bifunctional hydrogen peroxide sensor of electrogenerated chemiluminescence and Optical Electro-Chemistry of embodiment 2 preparation, its detecting step is:
(1) utilizing electrochemical workstation, adopt the method for step voltage that W1 applies step voltage on W1, initial voltage is 0v, and step voltage is 0.8v, and snap time is 20s；Meanwhile, when adopting on W2, W2 is applied constant voltage by m-current methods, and voltage is 0.3v；
(2) and (3) with embodiment 4.
Embodiment 6A kind of application based on the bifunctional hydrogen peroxide sensor of electrogenerated chemiluminescence and Optical Electro-Chemistry
A kind of detection being applied to hydrogen peroxide based on the bifunctional hydrogen peroxide sensor of electrogenerated chemiluminescence and Optical Electro-Chemistry of embodiment 3 preparation, its detecting step is:
(1) utilizing electrochemical workstation, adopt the method for step voltage that W1 applies step voltage on W1, initial voltage is 0v, and step voltage is 0.9v, and snap time is 30s；Meanwhile, when adopting on W2, W2 is applied constant voltage by m-current methods, and voltage is 0.6v；
(2) and (3) with embodiment 4.
Embodiment 7Hydrogen peroxide sensor prepared by embodiment 1-3, is applied to the detection of hydrogen peroxide, has excellent Detection results, and detection is limited to 25 μm of ol/L.
The detection of hydrogen peroxide in embodiment 8 human serum
Accurately pipette human serum sample, add the Hydrogen peroxide standard solution of certain molar concentration, with do not add hydrogen peroxide human serum for blank, carry out recovery testu, detecting according to the step of embodiment 4 ~ 6, measure the response rate of hydrogen peroxide in sample, testing result is in Table 1.
The testing result of hydrogen peroxide in table 1 human serum
Table 1 testing result is it can be seen that the relative standard deviation (RSD) of result is less than 3.0%, and the response rate is 95.2 ~ 104%, it was shown that the present invention can be used for the detection of hydrogen peroxide in human serum, and highly sensitive, the high specificity of method, result is accurately and reliably.
Claims (5)
1. the preparation method based on the bifunctional hydrogen peroxide sensor of electrogenerated chemiluminescence and Optical Electro-Chemistry, it is characterized in that, adopt the ITO electro-conductive glass that gold palladium nanometer rods Sol A uPdNRs and electropolymerization luminol are modified jointly as electrogenerated chemiluminescence working electrode W1, titanium dioxide nanoplate colloidal sol TiO2The ITO electro-conductive glass that NSs and horseradish peroxidase Solution H RP modifies 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 based on the bifunctional hydrogen peroxide sensor of electrogenerated chemiluminescence and Optical Electro-Chemistry.
2. preparation method according to claim 1, it is characterized in that, the aqueous solution of the described rod-like nano material that golden palladium nanometer rods Sol A uPdNRs is nucleocapsid structure, the rod-like nano material of described nucleocapsid structure is with gold nanorods for core, Pd nano particle is the rod-like nano material of shell, described gold nanorods is bar-like golden nanometer particle, and length is 20 ~ 40nm.
3. preparation method 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.
4. preparation method 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.
5. the hydrogen peroxide sensor that prepared by preparation method according to claim 1, it is characterized in that, described hydrogen peroxide sensor is applied to the step of hydrogen peroxide detection: utilize electrochemical workstation, W1 is applied step voltage by the method adopting step voltage on W1, initial voltage is 0v, step voltage is 0.7 ~ 0.9v, and snap time is 10 ~ 30s；Meanwhile, when adopting on W2, W2 is applied constant voltage by m-current methods, and voltage is 0 ~ 0.6v；Adding hydrogenperoxide steam generator to be measured in electrolyzer, the electric current on W2 can increase accordingly along with the increase of concentration of hydrogen peroxide, and increasing according to gained electric current is worth hydrogenperoxide steam generator concentration to be measured.
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| CN114113049A (en) * | 2021-11-30 | 2022-03-01 | 南京信息工程大学 | Preparation method and application of self-luminous photonic crystal electrochemiluminescence sensor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107008895A (en) * | 2017-04-12 | 2017-08-04 | 济南大学 | A kind of rhotanium nanometer rods with excellent near-infrared absorption and PhotoelectrocatalytiPerformance Performance and preparation method thereof |
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| CN111693516A (en) * | 2020-05-07 | 2020-09-22 | 四川轻化工大学 | Gas-liquid phase electrochemical luminescence detection device and detection method |
| CN114113049A (en) * | 2021-11-30 | 2022-03-01 | 南京信息工程大学 | Preparation method and application of self-luminous photonic crystal electrochemiluminescence sensor |
| CN114113049B (en) * | 2021-11-30 | 2023-05-30 | 南京信息工程大学 | Preparation method and application of self-luminous photonic crystal electrochemiluminescence sensor |
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