CN101587094A - Method for concurrent measurement of dopamine and ascorbic acid using glassy carbon electrode - Google Patents
Method for concurrent measurement of dopamine and ascorbic acid using glassy carbon electrode Download PDFInfo
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- CN101587094A CN101587094A CNA2009100520289A CN200910052028A CN101587094A CN 101587094 A CN101587094 A CN 101587094A CN A2009100520289 A CNA2009100520289 A CN A2009100520289A CN 200910052028 A CN200910052028 A CN 200910052028A CN 101587094 A CN101587094 A CN 101587094A
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Abstract
The invention relates to a method for modifying glassy carbon electrode using semi-conductor nano material zinc sulphide and measuring dopamine ascorbic acid at the same time, which belongs to the field of electrochemical analysis and detection technique. The invention principally uses semi-conductor nano material zinc sulphide alcohol fluid dispersion to drop on the glassy carbon electrode, thereby modifying the glassy carbon electrode and improving stability of surface of glassy carbon electrode. The method provided by the invention uses nano zinc sulphide to modify glassy carbon electrode, which is used as a novel electrochemical sensor, and is good for rapid electrochemical determination of dopamine and ascorbic acid at the same time.
Description
Technical field
The present invention relates to a kind of method of utilizing semiconductor nano material zinc sulphide modified glassy carbon electrode to measure dopamine and ascorbic acid simultaneously, belong to electrochemical analysis detection technique field.
Background technology
The semiconductor nano particulate is meant semiconductor nonmetal oxide, transition metal oxide and the transition metal of particle diameter between 1～100nm and the particulate of V～VII main group formation compound.The conductor nano material is owing to have optical nonlinearity and the luminosity that is different from the body material, its physical length is suitable with the electronics free path, the transport process of charge carrier will present significant quantum mechanics feature, mainly be small-size effect, surface and interfacial effect, quantum size effect and macroscopical tunnel effect etc., above-mentioned effect makes the Nano semiconductor device have unique and good light, electricity, heat and mechanical property.Nano particle has different characteristics such as high-specific surface area, high activity, strong absorption affinity and high catalytic efficiency, and nano particle is used as electrode active material, has given electrode the performance more superior than traditional electrode.Application with the semi-conductor nano particles modified electrode is rare.
Dopamine (DA) is a kind of important neurotransmitter, and the nervous centralis in running plays an important role in kidney and the internal system.The dopamine maladjusted nervous system is schizophrenia and Parkinsonian major reason in the brain.Therefore to the research of its assay method, to inquire into its give birth in the diagnosis of mechanism and relevant disease have great importance.Same, ascorbic acid is the vitamin in the human diet, is being used for the treatment of flu, mental disease, infertility, and cancer, acquired immune deficiency syndrome (AIDS) play an important role.
Dopamine and ascorbic acid high overpotential and oxidation peak on bare electrode is overlapped, and it can't directly be measured.There is current potential optionally accurately to measure the important topic that these two kinds of materials are Electroanalytical Chemistry, biology and medical research field.The galvanochemistry modified electrode can effectively reduce the overpotential of some material redox material, thereby reaches the purpose of separating and measuring.Assay method for dopamine and ascorbic acid has at present: chemoluminescence method, liquid chromatography, spectrophotometric method, fluorometry, gas chromatography-mass spectrography logotype and Capillary Electrophoresis etc.More than several assay methods to ascorbic acid and dopamine be not easy to carry, cost an arm and a leg complicated operation.According to the document of being consulted, though we find that present stage is more and more about the report of modified electrode, the whole bag of tricks of measuring ascorbic acid and dopamine about modified electrode is a lot, but we are with the nanometer-material-modified modified electrode of making electrode stability height, favorable reproducibility, also semiconductor nano material zinc sulphide modified glassy carbon electrode are not measured the bibliographical information of dopamine and ascorbic acid at present.
Summary of the invention
The purpose of this invention is to provide a kind of method of utilizing semiconductor nano material zinc sulphide modified glassy carbon electrode to measure dopamine and ascorbic acid simultaneously.
A kind of method of utilizing semiconductor nano material zinc sulphide modified glassy carbon electrode to measure dopamine and ascorbic acid simultaneously of the present invention is characterized in that having following process and step:
A. the preparation of semiconductor nano material zinc sulphide modified glassy carbon electrode
(1) at first will carry out surface finish as the vitreous carbon of electrode material and handle, make the formation minute surface, carry out ultrasonic cleaning with distilled water, watery hydrochloric acid, absolute ethyl alcohol and redistilled water successively subsequently, obtain clean glass-carbon electrode; Stand-by;
(2) preparation nano-sized carbon zinc sulphide dressing agent: take by weighing certain amount of nano zinc sulphide and be positioned in a certain amount of absolute alcohol solution, it is uniformly dispersed with ultrasound wave; The proportioning of the consumption of nano-zinc sulfide and absolute alcohol solution usage is measured with w/v (ml/mg), and promptly per 1 milligram of nano-zinc sulfide uses 0.2 milliliter absolute alcohol solution; Promptly make dressing agent;
(3) above-mentioned finely dispersed dressing agent is dripped on the glass-carbon electrode surface of above-mentioned cleaning, at room temperature dry; Put into phosphate buffered solution subsequently in pH=7.0; It is stable to be scanned up to figure with cyclic voltammetry then in the current potential meaning mouth of-0.2～0.8V; Rinse well with redistilled water again, promptly make semiconductor nano material zinc sulphide modified glassy carbon electrode;
B. measure dopamine and ascorbic acid simultaneously with the zinc sulphide modified glassy carbon electrode
As working electrode, contrast electrode is saturated and calomel electrode with semiconductor nano material zinc sulphide modified glassy carbon electrode, and auxiliary electrode is the platinized platinum electrode, forms three-electrode system; This three-electrode system placed to contain certain density ascorbic acid and dopamine and pH be 7.0 phosphate buffered solution; Then-0.2～0.8V cyclic voltammetry scan a few with activated electrode, carry out differential pulse volt-ampere dress afterwards, and note the I-E curve; On semiconductor nano material zinc sulphide modified glassy carbon electrode, two independently spikes appear in ascorbic acid and dopamine, peak resolution height, and the peak position difference reaches 0.2V, has realized measuring simultaneously dopamine and ascorbic acid.
The present invention utilizes nano particle to have the optics electrical properties of many uniquenesses, high specific surface area and other character relevant with size, after nano particle is handled through finishing and component control etc., be easy to and biomaterial coupling mutually, nano material itself is very stable, modify the modified electrode that obtains with nano material zinc sulphide, very strong stability is arranged.Semiconductor nano material zinc sulphide alcohol of the present invention disperses also can be dispersed in the surface of glass-carbon electrode, and the decorative layer of formation is more stable, helps carrying out in phosphate buffered solution voltammetric measuring.
Modified electrode among the present invention is a kind of novel electrochemical sensor, and the fast electrochemical that can be directly used in dopamine and ascorbic acid is measured, have fast, sensitive, accurately, characteristics such as catalytic height.Method of testing of the present invention has good stable and reappearance.Novel modified glassy carbon electrode its preparation method among the present invention is simple, quick, easy to operate, modifies mild condition.
Description of drawings
Fig. 1 is the dopamine and the ascorbic acid (5.0 * 10 of same concentrations among the present invention
-4M) figure of the differential pulse volt-ampere (I-E) on different electrode glass carbon bare electrodes (a), semiconductor nano material zinc sulphide modified glassy carbon electrode (b).
Fig. 2 is the dopamine of variable concentrations among the present invention and ascorbic acid the chlorination peak current in the differential pulse voltammogram and the linear relationship chart of concentration on semiconductor nano material sulfuration modified glassy carbon electrode.
Embodiment
Now specific embodiments of the invention are described in detail in after.
The process and the step of the assay method in the present embodiment are as follows:
(1) at first with glass-carbon electrode at 0.05 μ m Al
2O
3Be polished to minute surface on the polishing flannelet, then ultrasonic cleaning pre-service in distilled water, dilute nitric acid solution, absolute ethyl alcohol and redistilled water successively;
(2) preparation semiconductor nano material zinc sulphide modified glassy carbon electrode: the alcohol dispersion liquid that on the good glass-carbon electrode of pre-service, drips semiconductor nano zinc sulphide; The compound method of this dressing agent is: at first claim to remove the 50mg nano-zinc sulfide, place the absolute alcohol solution of 10ml, ultrasonicly be uniformly dispersed in alcohol to nano-zinc sulfide, obtain required dressing agent;
(3) a certain amount of above-mentioned finely dispersed dressing agent is dropped on the glass-carbon electrode matrix surface that cleans up, and at room temperature dry, put into phosphate buffered solution subsequently in pH=4.7; Then in the potential window of-0.2～0.8V cyclic voltammetry to be scanned up to figure stable; Rinse well with redistilled water again, promptly make semiconductor nano material zinc sulphide modified glassy carbon electrode:
(4) above-mentioned modified glassy carbon electrode is directly used in the electrochemical gaging of dopamine and ascorbic acid; Its assay method is as follows: as working electrode, contrast electrode is a saturated calomel electrode with semiconductor nano material zinc sulphide modified glassy carbon electrode, and auxiliary electrode is the platinized platinum electrode, forms three-electrode system; This three-electrode system placed to contain certain density ascorbic acid and dopamine and pH be 4.7 phosphate buffered solution; A few carry out the differential pulse voltammetry with activated electrode to current potential afterwards from-0.2V to+0.8V cyclic voltammetry scan, and record I-E curve; Illustrate at curve map, on semiconductor nano material zinc sulphide modified glassy carbon electrode, two independently spikes appear in ascorbic acid and dopamine, peak resolution height, and the spike potential difference reaches 0.2V; Dopamine and ascorbic acid have been realized measuring simultaneously.
Electrochemical gaging
1, the dopamine of same concentrations and ascorbic acid (5.0 * 10
-4M) the differential pulse voltammetric measuring on different electrodes adopts different electrodes, i.e. glass carbon bare electrode (a) and semiconductor nano material zinc sulphide modified glassy carbon electrode (b).
Test condition: with the glass-carbon electrode is working electrode, is contrast electrode with the saturated calomel electrode, is auxiliary electrode with the platinized platinum electrode; The concentration of dopamine and ascorbic acid is 5.0 * 10
-4M; End liquid is the 0.1M phosphate buffered solution of pH=7.0; Take-off potential is-0.2V that the termination current potential is 0.8V; Pulse increment is 0.001; Pulse height is 0.05; Pulse width is 0.04; Be 0.2S rest time; Sensitivity is 20 * 10
-6Sweep limit is-0.2～+ 0.8V.
Referring to Fig. 1, from the I-E curve of Fig. 1 as seen, a broad peak only appears in the melting concn of ascorbic acid and dopamine on glass carbon bare electrode; And on semiconductor nano material zinc sulphide modified glassy carbon electrode, two independently spikes appear in ascorbic acid and dopamine, peak resolution height, and the peak position difference reaches 0.2V.
2, exist under the condition of certain density dopamine, the ascorbic acid of variable concentrations is the differential pulse voltammetric measuring on semiconductor nano material zinc sulphide modified glassy carbon electrode
Adopting the volumetric molar concentration of ascorbic acid is 1.0～10
-4, 2.0～10
-4, 3.0～10
-4, 4.0～10
-4, 5.0～10
-4, 6.0～10
-4, 7.0～10
-4M; Adopt the volumetric molar concentration 2.0～10 of dopamine
-4M.
Test condition: with semiconductor nano material zinc sulphide modified glassy carbon electrode is working electrode, is contrast electrode with the saturated calomel electrode, is that auxiliary electrical extremely becomes three-electrode system with the platinized platinum; End liquid is the 0.1M phosphate buffered solution of pH=7.0.
Electricity is swept and is arranged a few with activated electrode from-0.2V to+0.8V cyclic voltammetric; Carry out the differential pulse voltammetric determination afterwards.
Referring to Fig. 2, Fig. 2 exists under the condition of certain density dopamine, the ascorbic acid of variable concentrations the oxidation peak value among the differential pulse figure and linear relationship chart of concentration on semiconductor nano material zinc sulphide modified electrode.Along with ascorbic acid concentrations increases, its oxidation peak current also increases.The linear relationship curve I of the bad hematic acid of hole that obtains
P=1.2157C+5.0687, linearly dependent coefficient R=0.9988.
Claims (1)
1, a kind of method of utilizing semiconductor nano material zinc sulphide modified glassy carbon electrode to measure dopamine and ascorbic acid simultaneously is characterized in that having following process and step:
A. the preparation of semiconductor nano material zinc sulphide modified glassy carbon electrode
(1) at first will carry out surface finish as the vitreous carbon of electrode material and handle, make the formation minute surface, carry out ultrasonic cleaning with distilled water, watery hydrochloric acid, absolute ethyl alcohol and redistilled water successively subsequently, obtain clean glass-carbon electrode; Stand-by;
(2) preparation nano-sized carbon zinc sulphide dressing agent: take by weighing certain amount of nano zinc sulphide and be positioned in a certain amount of absolute alcohol solution, it is uniformly dispersed with ultrasound wave; The proportioning of the consumption of nano-zinc sulfide and absolute alcohol solution usage is measured with w/v (ml/mg), and promptly per 1 milligram of nano-zinc sulfide uses 0.2 milliliter absolute alcohol solution; Promptly make dressing agent;
(3) above-mentioned finely dispersed dressing agent is dripped on the glass-carbon electrode surface of above-mentioned cleaning, at room temperature dry; Put into phosphate buffered solution subsequently in pH=7.0; It is stable to be scanned up to figure with cyclic voltammetry then in the current potential meaning mouth of-0.2～0.8V; Rinse well with redistilled water again, promptly make semiconductor nano material zinc sulphide modified glassy carbon electrode;
B. measure dopamine and ascorbic acid simultaneously with the zinc sulphide modified glassy carbon electrode
As working electrode, contrast electrode is saturated and calomel electrode with semiconductor nano material zinc sulphide modified glassy carbon electrode, and auxiliary electrode is the platinized platinum electrode, forms three-electrode system; This three-electrode system placed to contain certain density ascorbic acid and dopamine and pH be 7.0 phosphate buffered solution; Then-0.2～0.8V cyclic voltammetry scan a few with activated electrode, carry out differential pulse volt-ampere dress afterwards, and note the I-E curve; On semiconductor nano material zinc sulphide modified glassy carbon electrode, two independently spikes appear in ascorbic acid and dopamine, peak resolution height, and the peak position difference reaches 0.2V, has realized measuring simultaneously dopamine and ascorbic acid.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102288657A (en) * | 2011-07-09 | 2011-12-21 | 盐城工学院 | Method for detecting ascorbic acid with cysteine-modified polydimethylsiloxane-nano gold compound material |
| RU2610220C1 (en) * | 2015-11-18 | 2017-02-08 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский Томский государственный университет" (ТГУ, НИ ТГУ) | Method for determining ascorbic acid and dopamine in water at joint presence using modified electrodes |
| CN110376265A (en) * | 2019-08-15 | 2019-10-25 | 蚌埠学院 | A method of detection ascorbic acid |
| CN113466299A (en) * | 2020-09-22 | 2021-10-01 | 镇江宏祥自动化科技有限公司 | Electrochemical sensor for detecting ascorbic acid, uric acid and dopamine and preparation method thereof |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1201146C (en) * | 2002-07-18 | 2005-05-11 | 武汉大学 | Electrochemical sensor for determining dopamine |
| US20050244811A1 (en) * | 2003-12-15 | 2005-11-03 | Nano-Proprietary, Inc. | Matrix array nanobiosensor |
| JP2006053115A (en) * | 2004-08-11 | 2006-02-23 | Radiance Ware Kk | Electrode for measuring hydrogen peroxide and oxidase substrate |
| CN101149353A (en) * | 2007-09-06 | 2008-03-26 | 温州医学院 | Carbon nano tube/ overoxidation polypyrrole composite modified electrode preparation method and uses |
| CN101285793B (en) * | 2008-04-21 | 2012-03-28 | 上海大学 | Method for simultaneously determining dopamine and ascorbic acid by utilizing modified glassy carbon electrode |
-
2009
- 2009-05-26 CN CN2009100520289A patent/CN101587094B/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102288657A (en) * | 2011-07-09 | 2011-12-21 | 盐城工学院 | Method for detecting ascorbic acid with cysteine-modified polydimethylsiloxane-nano gold compound material |
| RU2610220C1 (en) * | 2015-11-18 | 2017-02-08 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский Томский государственный университет" (ТГУ, НИ ТГУ) | Method for determining ascorbic acid and dopamine in water at joint presence using modified electrodes |
| CN110376265A (en) * | 2019-08-15 | 2019-10-25 | 蚌埠学院 | A method of detection ascorbic acid |
| CN113466299A (en) * | 2020-09-22 | 2021-10-01 | 镇江宏祥自动化科技有限公司 | Electrochemical sensor for detecting ascorbic acid, uric acid and dopamine and preparation method thereof |
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| CN101587094B (en) | 2012-05-23 |
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