CN102539480A - Preparation method of amperometric glucose sensor based on highly-ordered titanium dioxide nanotube array - Google Patents
Preparation method of amperometric glucose sensor based on highly-ordered titanium dioxide nanotube array Download PDFInfo
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- CN102539480A CN102539480A CN2012100057212A CN201210005721A CN102539480A CN 102539480 A CN102539480 A CN 102539480A CN 2012100057212 A CN2012100057212 A CN 2012100057212A CN 201210005721 A CN201210005721 A CN 201210005721A CN 102539480 A CN102539480 A CN 102539480A
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Abstract
The invention discloses a preparation method of an amperometric glucose sensor based on a highly-ordered titanium dioxide nanotube array. The preparation method comprises the following steps of: 1) pretreating titanium; 2) oxidizing a titanium anode; 3) calcining a titanium wire with an oxidized anode at 300 DEG C to 500 DEG C for 1-3h for annealing treatment to obtain the highly-ordered titanium dioxide nanotube array; and 4) soaking the titanium dioxide nanotube array in glucose oxidase solution for 6-12h, cleaning, dripping Nafion solution on the surface for packaging and air-drying in 0-10 DEG C refrigerator. By using the high-specific-surface-area titanium dioxide nanotube array to load the glucose oxidase, the utilization ratio of the glucose oxidase is above 20 percent, the detection limit of the amperometric glucose sensor is low and reaches 2muM, the detection range is wide and is 0.25-2.5mM, the sensitivity is high and reaches 29.6muA/mM.CM<-2> and the utilization ratio and the catalytic activity of the oxidase can be improved. The amperometric glucose sensor has the advantages of low detection limit, wide detection range and high sensitivity.
Description
Technical field
The present invention relates to a kind of preparation method of the current mode glucose sensor based on the high-sequential Nano tube array of titanium dioxide, belong to the biosensor technology field.
Background technology
Glucose is the indispensable nutriment of biosome intracellular metabolic, and its oxidation liberated heat is the main source of biosome institute energy requirement.Along with growth in the living standard, the incidence of disease of diabetes is in rising trend, and therefore, development can detect the method for low concentration glucose quick, easy, delicately, is of great practical significance.
In recent years, glucose sensor has become a research direction of aspects such as biochemical analysis and clinical examination owing to highly sensitive, good stability, simple operation and other advantages.The method that present most glucose biological sensor is employed in the electrode face finish glucose oxidase prepares, in the hope of obtaining the sensor of high sensitivity and high selectivity.But glucose oxidase is soluble in water, and character is unstable, and the activated centre of enzyme is buried at protein interior, these factor affecting the sensitivity of glucose biological sensor, stability and reappearance, also limited its industrialized development.As a kind of novel bio-sensing medium, select suitable fixing means that it is combined with enzyme nano material, have great importance for the performance that improves biology sensor.The present invention utilizes the Nano tube array of titanium dioxide of high-sequential, improves the utilization factor and the catalytic activity of glucose oxidase, and prepared current mode glucose sensor detectability is low, highly sensitive, and manufacturing process simply is easy to realize industrialization.
Summary of the invention
The present invention provides a kind of preparation method of the current mode glucose sensor based on the high-sequential Nano tube array of titanium dioxide.Through the anodic oxidation of Titanium, on the titanium matrix, obtain the Nano tube array of titanium dioxide of high-sequential; Glucose oxidase is loaded on the Nano tube array of titanium dioxide, process the current mode electrochemical glucose sensor, realize effectively detecting fast glucose.
Technical scheme of the present invention is: a kind of preparation method of the current mode glucose sensor based on the high-sequential Nano tube array of titanium dioxide, and its step is following:
(1) pre-treatment of titanium: the titanium silk was put into the ultrasonic 10-15 of water, ethanol and acetone minute successively, etch 10-15 second in the red fuming nitric acid (RFNA), cleaned back nitrogen in the water and dash and do;
(2) titanium anodic oxidation: the titanium silk after will handling is put into NH
4In the ethylene glycol solution of F, platinized platinum or graphite are negative electrode, and the titanium silk is an anode, at room temperature carry out electrochemical polish with the constant current direct current of 20-60V, and polishing time is 0.5-3 hour;
(3) Nano tube array of titanium dioxide aftertreatment: the titanium silk after the anodic oxidation calcined under 300-500 ℃ condition carried out annealing in process in 1-3 hour, obtain the high-sequential Nano tube array of titanium dioxide;
(4) sensor production: Nano tube array of titanium dioxide was soaked in glucose oxidase solution 6-12 hour; Clean; The surface drips the encapsulation of Nafion solution, in 0-10 ℃ refrigerator, dries, and obtains the current mode glucose sensor based on titania nanotube.
NH in the said step (2)
4In the ethylene glycol solution of F, NH
4The concentration of F is 0.1-0.3 mol/L.
The concentration of glucose oxidase solution is 10-30g/L in the said step (4).
The invention has the beneficial effects as follows: the Nano tube array of titanium dioxide load glucose oxidase that utilizes high-ratio surface; The utilization factor of enzyme is more than 20%; Current mode glucose sensor detectability hangs down 2 μ M, the wide 0.25-2.5mM of sensing range, highly sensitive 29.6 μ A/mMcm
-2, can improve oxidasic utilization factor and catalytic activity, made current mode glucose sensor detectability is low, and sensing range is wide, and is highly sensitive, and manufacturing process simply is easy to realize industrialization.
Description of drawings
Fig. 1 is the FESEM figure of the Nano tube array of titanium dioxide of high-sequential.
Fig. 2 is that the sensor's response electric current is with the change curve of concentration of glucose in phosphate buffer (PBS).
Embodiment
Embodiment 1
A kind of preparation method of the current mode glucose sensor based on the high-sequential Nano tube array of titanium dioxide, its step is following:
(1) pre-treatment of titanium: the titanium silk was put into water, ethanol and acetone ultrasonic 10 minutes successively, and etch is 10 seconds in the red fuming nitric acid (RFNA), cleans back nitrogen in the water and dashes dried;
(2) titanium anodic oxidation: the titanium silk after will handling is put into NH
4In the ethylene glycol solution of F, NH
4The concentration of F is 0.1 mol/L, and platinized platinum or graphite are negative electrode, and the titanium silk is an anode, at room temperature carries out electrochemical polish with the constant current direct current of 20V, and polishing time is 0.5 hour;
(3) Nano tube array of titanium dioxide aftertreatment: the titanium silk after the anodic oxidation calcined under 300 ℃ condition carried out annealing in process in 1 hour, obtain the high-sequential Nano tube array of titanium dioxide;
(4) sensor production: Nano tube array of titanium dioxide was soaked in glucose oxidase solution 6 hours; The concentration of glucose oxidase solution is 10g/L; Clean; The surface drips the encapsulation of Nafion solution, in 0 ℃ refrigerator, dries, and obtains the current mode glucose sensor based on titania nanotube.
Embodiment 2
A kind of preparation method of the current mode glucose sensor based on the high-sequential Nano tube array of titanium dioxide, its step is following:
(1) pre-treatment of titanium: the titanium silk was put into water, ethanol and acetone ultrasonic 15 minutes successively, and etch is 15 seconds in the red fuming nitric acid (RFNA), cleans back nitrogen in the water and dashes dried;
(2) titanium anodic oxidation: the titanium silk after will handling is put into NH
4In the ethylene glycol solution of F, NH
4The concentration of F is 0.3 mol/L, and platinized platinum or graphite are negative electrode, and the titanium silk is an anode, at room temperature carries out electrochemical polish with the constant current direct current of 60V, and polishing time is 3 hours;
(3) Nano tube array of titanium dioxide aftertreatment: the titanium silk after the anodic oxidation calcined under 500 ℃ condition carried out annealing in process in 3 hours, obtain the high-sequential Nano tube array of titanium dioxide;
(4) sensor production: Nano tube array of titanium dioxide was soaked in glucose oxidase solution 12 hours; The concentration of glucose oxidase solution is 30g/L; Clean; The surface drips the encapsulation of Nafion solution, in 10 ℃ refrigerator, dries, and obtains the current mode glucose sensor based on titania nanotube.
Embodiment 3
A kind of preparation method of the current mode glucose sensor based on the high-sequential Nano tube array of titanium dioxide, its step is following:
(1) pre-treatment of titanium: the titanium silk was put into water, ethanol and acetone ultrasonic 12 minutes successively, and etch is 12 seconds in the red fuming nitric acid (RFNA), cleans back nitrogen in the water and dashes dried;
(2) titanium anodic oxidation: the titanium silk after will handling is put into NH
4In the ethylene glycol solution of F, NH
4The concentration of F is 0.2 mol/L, and platinized platinum or graphite are negative electrode, and the titanium silk is an anode, at room temperature carries out electrochemical polish with the constant current direct current of 40V, and polishing time is 2 hours;
(3) Nano tube array of titanium dioxide aftertreatment: the titanium silk after the anodic oxidation calcined under 400 ℃ condition carried out annealing in process in 2 hours, obtain the high-sequential Nano tube array of titanium dioxide;
(4) sensor production: Nano tube array of titanium dioxide was soaked in glucose oxidase solution 10 hours; The concentration of glucose oxidase solution is 20g/L; Clean; The surface drips the encapsulation of Nafion solution, in 5 ℃ refrigerator, dries, and obtains the current mode glucose sensor based on titania nanotube.
Embodiment 4
A kind of preparation method of the current mode glucose sensor based on the high-sequential Nano tube array of titanium dioxide, its step is following:
(1) pre-treatment of titanium: the titanium silk was put into the ultrasonic 10-15 of water, ethanol and acetone minute successively, etch 10-15 second in the red fuming nitric acid (RFNA), cleaned back nitrogen in the water and dash and do;
(2) titanium anodic oxidation: the titanium silk after will handling is put into NH
4In the ethylene glycol solution of F, NH
4The concentration of F is 0.1-0.3 mol/L, and platinized platinum or graphite are negative electrode, and the titanium silk is an anode, at room temperature carries out electrochemical polish with the constant current direct current of 20-60V, and polishing time is 0.5-3 hour;
(3) Nano tube array of titanium dioxide aftertreatment: the titanium silk after the anodic oxidation calcined under 300-500 ℃ condition carried out annealing in process in 1-3 hour, obtain the high-sequential Nano tube array of titanium dioxide;
(4) sensor production: Nano tube array of titanium dioxide was soaked in glucose oxidase solution 6-12 hour; The concentration of glucose oxidase solution is 10-30g/L; Clean; The surface drips the encapsulation of Nafion solution, in 0-10 ℃ refrigerator, dries, and obtains the current mode glucose sensor based on titania nanotube.
Claims (3)
1. preparation method based on the current mode glucose sensor of high-sequential Nano tube array of titanium dioxide is characterized in that its step is following:
(1) the titanium silk was put into the ultrasonic 10-15 of water, ethanol and acetone minute successively, etch 10-15 second in the red fuming nitric acid (RFNA), cleaned back nitrogen in the water and dash and do;
(2) the titanium silk after will handling is put into NH
4In the ethylene glycol solution of F, platinized platinum or graphite are negative electrode, and the titanium silk is an anode, at room temperature carry out electrochemical polish with the constant current direct current of 20-60V, and polishing time is 0.5-3 hour;
(3) the titanium silk after the anodic oxidation is calcined under 300-500 ℃ condition carried out annealing in process in 1-3 hour, obtain the high-sequential Nano tube array of titanium dioxide;
(4) Nano tube array of titanium dioxide was soaked in glucose oxidase solution 6-12 hour, clean, the surface drips the encapsulation of Nafion solution, in 0-10 ℃ refrigerator, dries, and obtains the current mode glucose sensor based on titania nanotube.
2. the preparation method of the current mode glucose sensor based on the high-sequential Nano tube array of titanium dioxide according to claim 1 is characterized in that: NH in the said step (2)
4In the ethylene glycol solution of F, NH
4The concentration of F is 0.1-0.3 mol/L.
3. the preparation method of the current mode glucose sensor based on the high-sequential Nano tube array of titanium dioxide according to claim 1 is characterized in that: the concentration of glucose oxidase solution is 10-30g/L in the said step (4).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104076077A (en) * | 2014-06-25 | 2014-10-01 | 东南大学 | Nitrogen doped titanium dioxide nanotube array enzyme electrode and preparation method and application thereof |
| CN107389733A (en) * | 2017-07-25 | 2017-11-24 | 电子科技大学 | A kind of hydrogen gas sensor of titanium silk based structures and preparation method thereof |
| CN113189158A (en) * | 2021-04-25 | 2021-07-30 | 武汉科技大学 | Hydrogen sulfide photoelectrochemical sensor and preparation method thereof |
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| CN101487814A (en) * | 2009-02-10 | 2009-07-22 | 扬州大学 | Production method for nano-gold glucose oxidase sensor with electronic medium as inclusion compound |
| US20090218234A1 (en) * | 2008-02-28 | 2009-09-03 | Shrisudersan Jayaraman | Methods Of Making Titania Nanostructures |
| CN101768771A (en) * | 2008-12-31 | 2010-07-07 | 北京大学 | Cylindrical and barrel-shaped titanium dioxide nanotube arrays and preparation method and application thereof |
| CN101896643A (en) * | 2007-07-26 | 2010-11-24 | 宾州研究基金会 | The Nano tube array of titanium dioxide of high-sequential |
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| CN101896643A (en) * | 2007-07-26 | 2010-11-24 | 宾州研究基金会 | The Nano tube array of titanium dioxide of high-sequential |
| US20090218234A1 (en) * | 2008-02-28 | 2009-09-03 | Shrisudersan Jayaraman | Methods Of Making Titania Nanostructures |
| CN101768771A (en) * | 2008-12-31 | 2010-07-07 | 北京大学 | Cylindrical and barrel-shaped titanium dioxide nanotube arrays and preparation method and application thereof |
| CN101487814A (en) * | 2009-02-10 | 2009-07-22 | 扬州大学 | Production method for nano-gold glucose oxidase sensor with electronic medium as inclusion compound |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104076077A (en) * | 2014-06-25 | 2014-10-01 | 东南大学 | Nitrogen doped titanium dioxide nanotube array enzyme electrode and preparation method and application thereof |
| CN107389733A (en) * | 2017-07-25 | 2017-11-24 | 电子科技大学 | A kind of hydrogen gas sensor of titanium silk based structures and preparation method thereof |
| CN107389733B (en) * | 2017-07-25 | 2020-05-12 | 电子科技大学 | Hydrogen sensor with titanium wire-based structure and preparation method thereof |
| CN113189158A (en) * | 2021-04-25 | 2021-07-30 | 武汉科技大学 | Hydrogen sulfide photoelectrochemical sensor and preparation method thereof |
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Application publication date: 20120704 |