CN104359961A - Sulfadiazine electrochemical sensor based on graphene modified electrode - Google Patents

Sulfadiazine electrochemical sensor based on graphene modified electrode Download PDF

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Publication number
CN104359961A
CN104359961A CN201410669123.4A CN201410669123A CN104359961A CN 104359961 A CN104359961 A CN 104359961A CN 201410669123 A CN201410669123 A CN 201410669123A CN 104359961 A CN104359961 A CN 104359961A
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China
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graphene
electrode
nafion
sulphadiazine
electrochemical sensor
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CN201410669123.4A
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Chinese (zh)
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马静颖
洪小平
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Zhejiang College of Construction
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Zhejiang College of Construction
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Abstract

The invention discloses a sulfadiazine electrochemical sensor based on a graphene modified electrode. The sensor consists of a graphene-Nafion-glassy carbon electrode, an Ag/AgCl (saturated KCL) reference electrode and a platinum wire auxiliary electrode, wherein the graphene-Nafion-glassy carbon electrode is prepared by the following steps: by using graphene as an electrode surface modifying material and taking a Nafion aqueous solution as a dispersant, ultrasonically shocking to prepare a uniform graphene-Nafion modifier; and preparing the graphene-Nafion-glassy carbon electrode by using a dispensing method. By using sulfadiazine as a probe molecule, a method for electrochemically detecting trace sulfadiazine by using the graphene-Nafion-glassy carbon electrode is researched and established. The sulfadiazine electrochemical sensor for drug detection has the advantages of being fast in response, good in stability, high in sensitivity, wide in linearity range and the like.

Description

A kind of sulphadiazine electrochemical sensor based on graphene modified electrode
Technical field
The present invention relates to the Graphene electrochemical sensor that a kind of trace sulphadiazine detects, be specifically related to prepare Graphene-Nafion-glass-carbon electrode, strengthen the electrochemical response of sulphadiazine, belong to amperometric electrochemical sensor field.
Background technology
   
Disulfonamide is a class broad spectrum antibiotic.Because low price, has a broad antifungal spectrum, is widely used in treatment and the control of Animal diseases in animal-breeding industry.Overdose or medication lack of standardization will to cause in animal derived product that antimicrobial is residual to exceed standard, and by food chain transport in consumer's body, harm humans is healthy.To detect in food that disulfonamide is residual to have important practical significance fast and accurately.
At present, the method such as in animal derived food, sulfa drug residue detection method mainly contains high performance liquid chromatography, euzymelinked immunosorbent assay (ELISA) (ELISA), chemoluminescence method, makings are used in conjunction.Although these method analysis results are sensitive, accurate, all belong to laboratory method, need main equipment, analysis cost is high.A kind of method finding disulfonamide that is sensitive, accurate, quick, that can be used for on-the site analysis to detect is particularly urgent.
Graphene has the advantages that specific surface area is large, good conductivity, catalytic activity are high, is suitable for very much design and prepares high-performance electric chemistry sensor, shows good effect for promoting the catalytic performance of electrochemical sensor, detection sensitivity and stability.
 
Summary of the invention
The object of the invention is to provide a kind of sulphadiazine electrochemical test sensors, for the Electrochemical Detection of trace sulphadiazine medicine, sets up trace sulfadiazine residue electrochemical detection method efficiently and effectively.
The present invention is achieved through the following technical solutions:
A kind of sulphadiazine electrochemical sensor based on graphene modified electrode, by Graphene-Nafion-glass-carbon electrode and the saturated KCl of Ag/AgCl() contrast electrode, platinum filament auxiliary electrode form, it is characterized in that: described Graphene-Nafion-glass-carbon electrode is prepared in the following way: take Graphene as electrode face finish material, with Nafion aqueous solution for spreading agent, ultrasonic oscillation process prepares uniform Graphene-Nafion dressing agent; Adopt drop-coating, prepare Graphene-Nafion-glass-carbon electrode.
Further, during use, supporting electrolyte used is dilution heat of sulfuric acid.
Further, detection method is used to be potentiostatic method.
Further, be 2.2x10 to the sensing range of sulphadiazine -7~ 8.7x10 -5mol/L, detects and is limited to 7.2x10 -8mol/L.
Further, responding required time is 2 seconds.
The present invention's proposition for dispersion solvent with Nafion aqueous solution, is prepared Graphene-Nafion dispersion soln, and is prepared Graphene-Nafion-glass-carbon electrode with drop-coating.Take sulphadiazine as probe molecule, research sets up Graphene-Nafion-glass-carbon electrode for the electrochemical method of trace sulphadiazine.Sulphadiazine drug test electrochemical sensor of the present invention has the advantages such as response is fast, good stability, highly sensitive, the range of linearity is wide.
Accompanying drawing explanation
Fig. 1 be in 0.1 mol/L dilution heat of sulfuric acid supporting electrolyte Different electrodes to the volt-ampere response diagram of 1.0 mmol/L sulphadiazines.
In Fig. 1, Reference numeral implication is:
1-Graphene-Nafion-glass carbon composite electrode; 2-carbon nano-tube-glass-carbon electrode; 3-Graphene-Nafion-glass carbon composite electrode is in blank solution; 4-glass-carbon electrode.
The constant potential response diagram of Fig. 2 Standard entertion sulphadiazine on Graphene-Nafion-glass-carbon electrode.
Fig. 3 constant potential response current-sulphadiazine concentration-response working curve diagram.
embodiment
Below in conjunction with accompanying drawing, the invention will be further described.
Sulphadiazine electrochemical sensor based on graphene modified electrode of the present invention, concrete preparation process is as follows:
1. take appropriate 5%(wt) Nafion solution (Aldrich), dilute 50 times with ultrapure water and obtain 0.1%(wt) Nafion aqueous solution.By appropriate graphene powder (Nanjing Ji Cang nanosecond science and technology company limited) ultrasound wave dispersion (10 min) in above-mentioned 0.1%(wt) obtain electrode modification liquid in Nafion lean solution, Graphene content is 0.5 mg/mL.
2., with drop-coating, get 4 μ L above-mentioned electrode modification drop and be added in clean glassy carbon electrode surface (Φ=3 mm, Shanghai Chen Hua Instrument Ltd.), volatilize solvent and obtain Graphene-Nafion-glass-carbon electrode.
3. with Graphene-Nafion-glass-carbon electrode for working electrode, Ag/AgCl (saturated KCl) contrast electrode, platinum filament auxiliary electrode, detects electrochemical sensor in conjunction with 5 mL glass electrolytic cells and 0.1 mol/L dilute sulfuric acid supporting electrolyte composition sulphadiazine.
4. with 0.1 mol/L dilution heat of sulfuric acid for supporting electrolyte, controlling potential 0.95 V potentiostatic deposition, record supporting electrolyte in sulphadiazine Faradaic current variation relation curve in time on a sensor, as shown in Figure 2; Working electrode constant potential response current and sulphadiazine concentration relationship working curve are as shown in Figure 3.
5. result display, the range of linearity detected sulphadiazine is 2.2x10 -7~ 8.7x10 -5mol/L, detects and is limited to 7.2x10 -8mol/L.

Claims (5)

1. the sulphadiazine electrochemical sensor based on graphene modified electrode, by Graphene-Nafion-glass-carbon electrode and the saturated KCl of Ag/AgCl() contrast electrode, platinum filament auxiliary electrode form, it is characterized in that: described Graphene-Nafion-glass-carbon electrode is prepared in the following way: take Graphene as electrode face finish material, with Nafion aqueous solution for spreading agent, ultrasonic oscillation process prepares uniform Graphene-Nafion dressing agent; Adopt drop-coating, prepare Graphene-Nafion-glass-carbon electrode.
2., as claimed in claim 1 based on the sulphadiazine electrochemical sensor of graphene modified electrode, it is characterized in that: during use, supporting electrolyte used is dilution heat of sulfuric acid.
3., as claimed in claim 1 based on the sulphadiazine electrochemical sensor of graphene modified electrode, it is characterized in that: use detection method is potentiostatic method.
4. as claimed in claim 1 based on the sulphadiazine electrochemical sensor of graphene modified electrode, it is characterized in that: be 2.2x10 to the sensing range of sulphadiazine -7~ 8.7x10 -5mol/L, detects and is limited to 7.2x10 -8mol/L.
5. as claimed in claim 1 based on the sulphadiazine electrochemical sensor of graphene modified electrode, it is characterized in that: response required time is 2 seconds.
CN201410669123.4A 2014-11-21 2014-11-21 Sulfadiazine electrochemical sensor based on graphene modified electrode Pending CN104359961A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106018533A (en) * 2016-07-01 2016-10-12 肇庆学院 Molecularly imprinted electrochemical sensor for detecting trace sulfamonomethoxine
CN106404864A (en) * 2016-11-04 2017-02-15 北京农业信息技术研究中心 Method for detecting methyl jasmonate in plants on basis of microelectrode biosensing technique
CN107966484A (en) * 2017-12-05 2018-04-27 南京师范大学淮安研究院 Application of the electrochemical immunosensor in sulphonamides multi-relict context of detection
CN112903773A (en) * 2021-01-19 2021-06-04 江西农业大学 Preparation method and application of hollow gold nanoshell modified flexible laser-induced graphene electrode

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103983673A (en) * 2014-05-21 2014-08-13 浙江建设职业技术学院 Electrochemical sensor for sulfamido compound detection and preparation method and application thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103983673A (en) * 2014-05-21 2014-08-13 浙江建设职业技术学院 Electrochemical sensor for sulfamido compound detection and preparation method and application thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
XIAO-PING HONG等: ""Electrochemical study of sulfadiazine on a novel phthalocyanine-containing chemically modified electrode"", 《CHINESE CHEMICAL LETTERS》 *
李焘等: ""纳米石墨烯修饰电极电化学发光法测定盐酸氯丙嗪的研究"", 《分析测试学报》 *
洪小平等: ""磺胺在多壁碳纳米管修饰铂电极上的伏安法测定"", 《科技通报》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106018533A (en) * 2016-07-01 2016-10-12 肇庆学院 Molecularly imprinted electrochemical sensor for detecting trace sulfamonomethoxine
CN106404864A (en) * 2016-11-04 2017-02-15 北京农业信息技术研究中心 Method for detecting methyl jasmonate in plants on basis of microelectrode biosensing technique
CN106404864B (en) * 2016-11-04 2018-12-25 北京农业信息技术研究中心 Plant methyl jasmonate detection method based on microelectrode biosensing technology
CN107966484A (en) * 2017-12-05 2018-04-27 南京师范大学淮安研究院 Application of the electrochemical immunosensor in sulphonamides multi-relict context of detection
CN112903773A (en) * 2021-01-19 2021-06-04 江西农业大学 Preparation method and application of hollow gold nanoshell modified flexible laser-induced graphene electrode

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