CN104076072A - High-sensitivity photoelectrochemical sensor made from iridium oxide-ferriporphyrin-titanium oxide and preparation method for sensor - Google Patents
High-sensitivity photoelectrochemical sensor made from iridium oxide-ferriporphyrin-titanium oxide and preparation method for sensor Download PDFInfo
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Abstract
The invention belongs to the technical field of photoelectrochemical sensors, and in particular relates to a high-sensitivity glutathione photoelectrochemical sensor made from iridium oxide-ferriporphyrin-titanium oxide and a preparation method for the sensor. The photoelectrochemical sensor takes an iridium oxide-ferriporphyrin-titanium oxide nano wire array as a working electrode, an Ag/AgCl electrode as a reference electrode and a platinum wire as a counter electrode; a PBS (phosphate buffer solution) with the pH of 7.4 is used as reaction electrolyte; the irradiation light intensity is equal to the sunshine, and the irradiation sectional area is 0.02-0.06cm<2>; the lowest sensitivity is 10nM. The preparation method comprises the steps of preparing a titanium oxide nano wire by adopting a hydrothermal method, bonding upper ferriporphyrin through chemical coupling, finally performing chemical immersion deposition on iridium oxide to prepare the iridium oxide-ferriporphyrin-titanium oxide nano wire array, and then preparing the photoelectrochemical sensor. The raw materials of the photoelectrochemical sensor are readily available; the preparation method is simple, environmentally-friendly, low in cost, high in response speed, large in linear range, high in selectivity and favorable for popularization and application.
Description
Technical field
The invention belongs to Optical Electro-Chemistry sensor technical field, be specifically related to a kind of high sensitivity glutathione Optical Electro-Chemistry sensor and preparation method thereof.
Background technology
Optical Electro-Chemistry process refers to the photoelectric conversion process shifting via electron excitation and electric charge that photochromics occurs under illumination effect.Electrochemica biological sensor, as independently integrated detecting device of one, has produced on biochemical, medical field the impact becoming more and more important.Along with the fast development of nanometer technology and materials chemistry, on the basis of the combination of Optical Electro-Chemistry process and electrochemica biological sensor, develop New Generation Optical galvanochemistry (PEC) bio-sensing, thereby learned to interact a kind of new Sensitive Detection method is provided for exploring different kind organism.In essence, and other analytical technology of having set up is as electrogenerated chemiluminescence (ECL)-sample, and it is also a kind of based on the electrochemical analytical technology of tradition that PEC analyzes.Therefore, the method has been inherited the latter's plurality of advantages, and as cheap, equipment is simple, highly sensitive.But, also there is very large difference between the two, PEC sensing technology has advantages of that some are difficult to realize in traditional electrical chemical platform.In Optical Electro-Chemistry detects, light is used as excitation signal and carrys out exciting light electrochemical substance, and electric signal is as detection signal, and this process is just in time contrary with ECL.Owing to having adopted two kinds of multi-form exciting and detection signal, this technical background signal is lower, therefore have very high sensitivity.In fact,, in the time using same design to carry out same substance detection, the method based on PEC is also than present better detection performance (as lower detectability) based on electrochemical method.
Optical Electro-Chemistry bioanalysis is a kind of analytical approach that newly occurs in recent years and develop rapidly, and it detects that principle is based on the bio-identification effect between recognition component and target molecule under illumination and the change that produces corresponding electric signal.Because the advantage that it is unique and the potentiality in following bio-sensing thereof, the method has attracted increasing concern, and has also obtained very much progress at aspects such as detecting performance and bio-sensing application.But, although the method has represented outstanding advantage in the work of having reported, in fact, industry to the research of Optical Electro-Chemistry bioanalysis also still in the starting stage.Especially,, compared with traditional electrical chemical method and optical analysis method, the detecting pattern of Optical Electro-Chemistry analytical approach and signal conduction mechanism wait further investigation and expansion.Therefore, development Optical Electro-Chemistry bioanalysis new method is necessary, and can provide novel and blanket path for following Optical Electro-Chemistry bioanalysis.This paper is prepared novel photoelectric chemical system and is explored new signal conduction mechanism by design, has successfully set up multiple Optical Electro-Chemistry bioanalysis new method, for further exploitation and the utilization of Photoelectrochemistrbiosensor biosensor are laid a good foundation.
Develop into now from the initial conditions of PEC bio-sensing, people have designed multiple sensors and have been used for detecting all types of target analyte.But for typical PEC bio-sensing, two core elements are indispensable, that is: photoelectric activity material (being used for producing detection signal) and biological identification element (being closely connected with electrode).As in the biology sensor of many other types, biological identification element part comprises: enzyme, antibody, nucleic acid etc.And for photoelectric activity material, more use be organic/inorganic semiconductor, such as ruthenium dipyridine and CdS quantum dot (QDs).The photon energy absorbing when semi-conductor nano particles is during higher than its band gap, and electronics transits to conduction band from valence band, has therefore produced electron hole pair.Once this charge transfer process occurs, the compound or electric charge that electron hole pair very easily occurs thereupon shifts.Under certain condition, conduction band electron can shift to the electron accepter in electrode or solution, thereby produces male or female photocurrent response.Meanwhile, valence band hole by be transferred to semiconductor material surface so that by the electron institute quencher from solution or electrode.The existence of effective electron donor/acceptor can efficiently suppress the compound of electron hole pair, promotes the stable generation of photocurrent.On the basis of being combined with biological identification element at photoelectric activity material, the principle of work of all PEC bio-sensings is all that the signal intensity of the current/voltage based on by electrode is monitored corresponding bio-identification reaction.Particularly, biological recognition system changes certain biochemical information (concentration of for example analyte) into the variation of certain specific factor of electrode surface (or around), and this variation meeting has close relationship with the performance of photoelectric activity material.Under illumination condition, electrode can interact the physical/chemical between biological recognition system and photoelectric activity material to be converted into electric signal subsequently.
Optical Electro-Chemistry detection method is the biomolecule detection technology that a kind of new development is got up, and owing to combining optical radiation and electrochemical detection method, Photoelectrochemistrbiosensor biosensor has advantages of optical means and electrochemical sensor simultaneously.Therefore this technology has represented good analytical applications prospect and has attracted to study widely interest.Some metal-oxide semiconductor (MOS) nano particles are such as ZnO, ZrO
2and TiO
2deng becoming generally acknowledged good Optical Electro-Chemistry material.Wherein, TiO
2nano particle has broad-band gap because of it, the active and powerful oxidability in the time exciting of high Optical Electro-Chemistry under ultraviolet lighting and being furtherd investigate, and be applied in the multiple approach based on Optical Electro-Chemistry.Excite TiO
2the photoelectric response producing has been applied in the design of Optical Electro-Chemistry sensor.Recently organic aptamers molecule that, important being used for of this class of porphyrin absorbs luminous energy has been widely used in improving molecular electronic device and especially solar cell TiO of photoelectric device
2the electricity conversion of nano particle.But this improved method that has improved electricity conversion is not also applied on the structure of Optical Electro-Chemistry bioanalytical sensing platform.Porphyrin Molecule shows swift electron and injects, and slower electric charge is composite moving mechanics character again, the performances such as high-level efficiency light absorption and good chemical stability.Some can be easy to be combined in TiO in the mode of coordination bond with carboxyl or sulfonic porphyrin
2on nano particle.A kind of zinc protoporphyrin sensitization TiO
2solar cell photoelectric transformation efficiency maximum can reach 65%, and corresponding energy conversion efficiency is 3.1% to the maximum.In addition, porphyrin and titanium dioxide surface exist stronger electricity right, because electronics is injected into from excited singlet porphyrin that to be excited the efficiency of titania conduction band very high in sensitization compound.In order to apply these advantages of titanium dioxide nano-particle of porphyrin functionalization, prepare the titanium dioxide nano-particle of FeTPPS sensitization by its sulfonic group and titania coordination with water-soluble FeTPPS.This nano-complex shows stable Optical Electro-Chemistry response, this response signal can be carried out electronic injection to porphyrin by biomolecule and is then injected into the titania exciting and further strengthen, and has therefore set up an Optical Electro-Chemistry bioanalytical sensing platform that novel application is very strong.For example it can successfully detect glutathione (GSH).
GSH, as a kind of thio-alcohol material extensively existing in vivo, is playing the part of important role in increasing many biochemical processes such as anti-oxidant, signal transduction, cell.A lot of diseases such as its content in vivo and cancer, acquired immune deficiency syndrome (AIDS), degeneration sacred disease, Alzheimer disease, Parkinson's disease have close relationship.Therefore the content tool that detects GSH under physiological environment is of great significance.The detection of GSH is proposed to a lot of methods, comprised microchip electrophoresis one laser inductive fluorescence method, quanta point electroluminescent method, absorption spectroscopy, fluorescent spectrometry, Surface Enhanced Raman Scattering Spectrum method, laser desorption ionization mass spectra method etc.The method of a series of Electrochemical Detection GSH is also developed, but the too high oxidizing potential using while detecting has limited the practical application of these electrochemical methods.FeTPPS-TiO
2under+0.2V current potential, can produce Optical Electro-Chemistry response to GSH, GSH is detected and is achieved under electronegative potential based on this, and this sensor shows the series of advantages such as quick, the wide range of linearity, high selectivity when GSH is detected, successfully apply to detect the glutathione content in tumour cell and normal cell.The titanium dioxide nano-particle of porphyrin functionalization provides brand-new approach for Photoelectric Detection biomolecule.
Yttrium oxide is catalyzer, has promoted to catch the ability in hole and has promoted to produce oxygen, and therefore we have prepared a kind of high sensitivity glutathione Optical Electro-Chemistry transducer production method of novel yttrium oxide-iron porphyrin-titanium dioxide, and are applied in life analyzing and testing.
Summary of the invention
The object of this invention is to provide high sensitivity glutathione Optical Electro-Chemistry sensor of a kind of novel yttrium oxide-iron porphyrin-titanium dioxide and preparation method thereof.
The high sensitivity glutathione Optical Electro-Chemistry sensor of yttrium oxide-iron porphyrin-titanium dioxide provided by the invention, taking yttrium oxide-iron porphyrin-TiOx nano linear array as working electrode, Ag/AgCl electrode is contrast electrode, platinum filament is to electrode, pH7.4 PBS solution is reaction electrolytic solution, light irradiation intensity is a sunshine, and irradiating sectional area is 0.02-0.06 cm
2.
The high sensitivity glutathione Optical Electro-Chemistry sensor of yttrium oxide-iron porphyrin-titanium dioxide provided by the invention, preparation method, concrete steps are:
(1) water is mixed to 0.1 – with concentrated acid after 0.5 hour, add wherein titanium source, Xi Yuan, under stirring, react 5 – 10 min, then transfer in reactor, the substrate front surface of suitable size is put into still down, under 140 180 DEG C of – conditions, react 4 – 20 hours;
(2) product above-mentioned steps being made is rinsed well, is dried, roasting 1 – 2 hours under 550 DEG C of temperature conditions of 450 – in air atmosphere, then roasting 0.5 – 2 hours under 550 DEG C of temperature conditions of 350 – in inert gas and reducibility gas mixed atmosphere, can obtain and mix titanium dioxide nanowire array;
(3) above-mentioned titanium dioxide nanowire array is placed in to concentrated acid soaked overnight, makes hydroxyl on its surface band;
(4) glass sheet N
2dry up, in silylating reagent 5% APTES ethanolic solution ultrasonic 1.5-2.5 hour (as 2 hours), N
2dry up, in 110-130 DEG C of baking ovens, toast 25-35 min(as toasted 30 min in 120 DEG C of baking ovens) make amino be modified at more securely titanium dioxide nano thread surface;
(5) glass sheet is put in to 1-2mg/mL(as 1.5 mg/mL) iron porphyrin DMSO solution in, and add under the participation of EDC and NHS chemical coupling agent, first ultrasonic 25-35min(is as 30 min), rear standing 20-30 hour (as 24 hours), glass sheet N
2dry up rear stand-by;
(6) preparation 25-35 mL(is as 30 mL), 0.8-1.2 mM(as 1 mM) the sour sodium hexahydrate of hexachloro iridium (IV), add wherein 0.2-0.4 mL(as 0.3 mL) 0.08-0.12 M(as 0.1 M) potassium hydroxide, be placed on heating plate and heat, in the time that becoming transparent violet color, solution colour stops heating, at this moment 4-6 times (as 5 times) dilute the solution of above-mentioned preparation, synthetic glass sheet in step (5) is put in solution and is soaked repeatedly, pure water cleans repeatedly, 65-75 DEG C (m is as 70 DEG C) dry, obtain yttrium oxide-iron porphyrin-TiOx nano linear array,
(7) taking yttrium oxide-iron porphyrin-TiOx nano linear array as working electrode, Ag/AgCl electrode is contrast electrode, and platinum filament is to electrode, and pH7.4 PBS solution is reaction electrolytic solution, light irradiation intensity is a sunshine, irradiates sectional area at 0.02-0.06 cm
2in scope, regulate.
Described concentrated acid soaks for the concentrated sulphuric acid or red fuming nitric acid (RFNA).
Described porphyrin is one or more in zinc protoporphyrin, manganoporphyrin, iron porphyrin, copper porphyrin and cobalt porphyrin.
Described iridium source is iridium dioxide, iridium black or iridous oxide.
Described silane is 3-aminopropyl triethoxysilane or aminopropyl trimethoxysilane.
In the present invention, in the high sensitivity glutathione Optical Electro-Chemistry sensor of yttrium oxide-iron porphyrin-titanium dioxide, mixing tin amount is gross mass 0.5 – 2%.Mix tin titanium dioxide nanowire array and can utilize the hydrogen manufacturing simultaneously of sun power photodissociation water generates photocurrent.
The high sensitivity glutathione Optical Electro-Chemistry sensor of yttrium oxide-iron porphyrin-titanium dioxide provided by the invention, its sensitivity minimization is 10 nM.Can be applicable in life analysis.Identification and the detection of Optical Electro-Chemistry sensor of the present invention to glutathione, has high sensitivity and low detectability, can detect 8000/mL HeLa cell, 5000/mL 293T cells simultaneously.Starting material wide material sources of the present invention, preparation method is simple, environmental protection, cheap, responds quick, the wide range of linearity, high selectivity, is conducive to apply.
Yttrium oxide-iron porphyrin of the present invention-titanium dioxide array is that first hydro-thermal method is prepared titanium oxide nano wire, by iron porphyrin on chemical coupling bonding, finally deposits yttrium oxide by chemical immersion.It is simple that yttrium oxide-iron porphyrin-TiOx nano linear array has manufacture craft, cost is low, good stability, high sensitivity and low detectability environment amenable feature, being applicable to large area produces, for significant on Optical Electro-Chemistry ability sensor research, also there is good prospect in photoelectricity bioanalysis field.
Brief description of the drawings
Fig. 1: a is yttrium oxide-iron porphyrin-titanium dioxide array SEM photo; B is yttrium oxide-iron porphyrin-titanium dioxide TEM photo.
Fig. 2: a is that photocurrent improves along with the amount of the external glutathione adding has progressively, and presents the variation of step; B is the concentration of matching and the curve map of photocurrent.
Fig. 3 is the high sensitivity glutathione Optical Electro-Chemistry sensor diagram of yttrium oxide-iron porphyrin-titanium dioxide.
Embodiment
Below, by following examples, the invention will be further described, and it will contribute to understand the present invention, but do not limit content of the present invention.
Under hydrothermal system, taking tetra-n-butyl titanate as titanium source, water is solvent, and butter of tin is Xi Yuan, the speed of concentrated hydrochloric acid regulation and control hydrolysis reaction, containing the titanium dioxide nanowire array of growing in the substrate of fluorine tin oxide (FTO) electro-conductive glass, then annealing in process titanium dioxide nano thread in air, by the processing of titanium dioxide nano thread sulfuric acid soaked overnight clear water, connects hydroxyl, by silane coupled upper iron porphyrin, then by the upper yttrium oxide nano particle of chemical immersion method deposition.The present invention is coupled traditional photodissociation water technology and biosensor technology, has improved the absorption efficiency of solar cell to light, has realized a one-step process of efficient photolysis water hydrogen and photoelectric conversion high sensitivity identification glutathione molecule generation photocurrent.Concrete operations are as follows:
First FTO glass is placed in to the reactor of 50 ml, face down, gets 15 ml water and mixes with 13 ml concentrated hydrochloric acids, then to adding 0.4 ml tetra-n-butyl titanate in it.Treat that solution stirs 5 – 10 minutes, after mixing, pour in reactor, under 150 DEG C of conditions, react 12 hours.After reaction finishes, substrate is taken out and cleans and dry up.Then, substrate is placed in tubular furnace under 450 DEG C of conditions to roasting 2 hours, titanium dioxide nanowire array is placed in to concentrated acid soaked overnight, make hydroxyl on its surface band; Glass sheet dries up with N2, and in silylating reagent 5% APTES ethanolic solution ultrasonic 2 hours, N2 dried up, and in 120 DEG C of baking ovens, toasts 30 min, makes amino be modified at more securely titanium dioxide nano thread surface; Glass sheet is put in the iron porphyrin DMSO solution of 1.5 mg/mL, and adds under the participation of EDC and NHS chemical coupling agent, first ultrasonic 30 min, rear standing 24h.Glass sheet dries up rear stand-by with N2; Prepare 30 mL, the sour sodium hexahydrate of 1 mM hexachloro iridium (IV), add wherein the 0.1 M potassium hydroxide of 0.3 mL, be placed on heating plate and heat, in the time that solution colour becomes transparent violet color, stop heating, at this moment the solution of 5 times of above-mentioned preparations of dilution, is put in glass sheet synthetic in (5) in solution and soaks repeatedly, pure water cleans 3 times, and 70 DEG C of oven dry can be used.
As shown in Figure 3, taking yttrium oxide-iron porphyrin-titanium dioxide as working electrode, Ag/AgCl electrode is contrast electrode, and platinum filament is to electrode, and pH 7.4 PBS solution are reaction electrolytic solution,, light irradiation intensity is a sunshine, irradiated area is 1 cm
2.Under 0.2 V condition, survey its photoelectricity flow valuve along with the time change (as Fig. 2 a), and matching the change curve of concentration and photocurrent (as Fig. 2 b).
Claims (6)
1. the high sensitivity glutathione Optical Electro-Chemistry sensor of a yttrium oxide-iron porphyrin-titanium dioxide, it is characterized in that taking yttrium oxide-iron porphyrin-TiOx nano linear array as working electrode, Ag/AgCl electrode is contrast electrode, platinum filament is to electrode, pH7.4 PBS solution is reaction electrolytic solution, light irradiation intensity is a sunshine, and irradiating sectional area is 0.02-0.06 cm
2; Sensitivity minimization is 10 nM.
2. a preparation method for the high sensitivity glutathione Optical Electro-Chemistry sensor of yttrium oxide-iron porphyrin-titanium dioxide as claimed in claim 1, is characterized in that concrete steps are:
(1) water is mixed to 0.1 – with concentrated acid after 0.5 hour, add wherein titanium source, Xi Yuan, under stirring, react 5 – 10 min, then transfer in reactor, the substrate front surface of suitable size is put into still down, under 140 180 DEG C of – conditions, react 4 – 20 hours;
(2) product above-mentioned steps being made is rinsed well, is dried, roasting 1 – 2 hours under 550 DEG C of temperature conditions of 450 – in air atmosphere, then roasting 0.5 – 2 hours under 550 DEG C of temperature conditions of 350 – in inert gas and reducibility gas mixed atmosphere, can obtain and mix titanium dioxide nanowire array;
(3) above-mentioned titanium dioxide nanowire array is placed in to concentrated acid soaked overnight, makes hydroxyl on its surface band;
(4) glass sheet N
2dry up ultrasonic 1.5-2.5 hour in silylating reagent 5% APTES ethanolic solution, N
2dry up, in 110-130 DEG C of baking ovens, toast 25-35 min and make amino be modified at more securely titanium dioxide nano thread surface;
(5) glass sheet is put in the iron porphyrin DMSO solution of 1-2mg/mL, and adds under the participation of EDC and NHS chemical coupling agent, first ultrasonic 25-35min, rear standing 20-30 hour, glass sheet N
2dry up rear stand-by;
(6) the sour sodium hexahydrate of 0.8-1.2 mM hexachloro iridium (IV) of preparation 25-35 mL, add wherein the 0.08-0.12 M potassium hydroxide of 0.2-0.4 mL, be placed on heating plate and heat, in the time that becoming transparent violet color, solution colour stops heating, at this moment 4-6 doubly dilutes the solution of above-mentioned preparation, synthetic glass sheet in step (5) is put in solution and is soaked repeatedly, pure water cleans repeatedly, 65-75 DEG C of oven dry, obtains yttrium oxide-iron porphyrin-TiOx nano linear array;
(7) taking yttrium oxide-iron porphyrin-TiOx nano linear array as working electrode, Ag/AgCl electrode is contrast electrode, and platinum filament is to electrode, and pH7.4 PBS solution is reaction electrolytic solution, and light irradiation intensity is a sunshine, irradiates sectional area at 0.02-0.06 cm
2in scope, regulate.
3. preparation method as claimed in claim 2, is characterized in that described concentrated acid is the concentrated sulphuric acid or red fuming nitric acid (RFNA).
4. preparation method as claimed in claim 2, is characterized in that described porphyrin is one or more in zinc protoporphyrin, manganoporphyrin, iron porphyrin, copper porphyrin and cobalt porphyrin.
5. preparation method as claimed in claim 2, is characterized in that described iridium source is iridium dioxide, iridium black or iridous oxide.
6. preparation method as claimed in claim 2, is characterized in that described silane is 3-aminopropyl triethoxysilane or aminopropyl trimethoxysilane.
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| CN104865299A (en) * | 2015-05-16 | 2015-08-26 | 济南大学 | Preparation method and application of nanometer gold palladium/3aminopropyl triethoxy silanization manganic oxide PSA (prostate-specific antigen) sensor |
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| CN107490652A (en) * | 2017-08-04 | 2017-12-19 | 中国科学院广州能源研究所 | A kind of single-orientated yttrium oxide nano-array prepares and the construction method of membrane electrode |
| CN109540989A (en) * | 2018-11-19 | 2019-03-29 | 清华-伯克利深圳学院筹备办公室 | A kind of sensitive electrode, preparation method and biosensor and its application using it |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104865299A (en) * | 2015-05-16 | 2015-08-26 | 济南大学 | Preparation method and application of nanometer gold palladium/3aminopropyl triethoxy silanization manganic oxide PSA (prostate-specific antigen) sensor |
| CN105699645A (en) * | 2016-02-25 | 2016-06-22 | 济南大学 | Application and preparation method of electrochemical salbutamol sensor |
| CN107490652A (en) * | 2017-08-04 | 2017-12-19 | 中国科学院广州能源研究所 | A kind of single-orientated yttrium oxide nano-array prepares and the construction method of membrane electrode |
| CN107490652B (en) * | 2017-08-04 | 2019-09-06 | 中国科学院广州能源研究所 | A kind of construction method of single-orientated yttrium oxide nano-array preparation and membrane electrode |
| CN109540989A (en) * | 2018-11-19 | 2019-03-29 | 清华-伯克利深圳学院筹备办公室 | A kind of sensitive electrode, preparation method and biosensor and its application using it |
| CN110006970A (en) * | 2019-05-10 | 2019-07-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of electrochemical sensor for dopamine detection and products thereof and application |
| CN110006970B (en) * | 2019-05-10 | 2021-06-04 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of electrochemical sensor for dopamine detection, product and application thereof |
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