CN108152346A - The preparation method and application of norfloxacin molecular imprinted electrochemical sensor based on nanometer modified by silver - Google Patents
The preparation method and application of norfloxacin molecular imprinted electrochemical sensor based on nanometer modified by silver Download PDFInfo
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- CN108152346A CN108152346A CN201711332346.1A CN201711332346A CN108152346A CN 108152346 A CN108152346 A CN 108152346A CN 201711332346 A CN201711332346 A CN 201711332346A CN 108152346 A CN108152346 A CN 108152346A
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- norfloxacin
- silver
- electrode
- phenylenediamine
- molecular imprinted
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
Abstract
The invention discloses a kind of preparation method and applications of the norfloxacin molecular imprinted electrochemical sensor based on nanometer modified by silver, nano silver colloidal sol is uniformly applied on the glass-carbon electrode of pretreatment first, then using o-phenylenediamine as function monomer, Norfloxacin is as template molecule, norfloxacin molecular imprinted o-phenylenediamine thin polymer film is obtained on the glass-carbon electrode of nanometer modified by silver by electrochemical polymerization, Norfloxacin template molecule is removed from norfloxacin molecular imprinted o-phenylenediamine thin polymer film again and obtains the norfloxacin molecular imprinted electrochemical sensor based on nanometer modified by silver.The norfloxacin molecular imprinted electrochemical sensor of nanometer modified by silver produced by the present invention has the linear detection range of non-constant width；The sensitivity of sensor is substantially increased, reduces detection limit；The electrochemical sensor high selectivity, strong antijamming capability；The method of the present invention is simple, of low cost, simple and efficient to sample detection.
Description
Technical field
The invention belongs to electrochemical sensor technology fields, and in particular to a kind of Norfloxacin based on nanometer modified by silver point
The preparation method and application of sub- trace electrochemical sensor.
Background technology
Norfloxacin is third generation fluoroquinolones broad spectrum antibiotic, and bacterium is prevented by the effect for interfering DNA gyrases
Chromosome replication can be effectively inhibited for gram-positive bacteria, negative microbial infections, be widely used in treat stomach, uropoiesis,
The diseases such as respiratory tract, glasses and skin infection.But toxic side effect there are many Norfloxacins is had been found that in clinical trial,
Stomach and central nervous system can be upset, cause lather, hallucinate, nympholepsy, depression, insomnia, suicide, can also
Lead to fetal anomaly, damage renal function etc..The production of antibody-resistant bacterium can be brought in poultry farming using Norfloxacin antimicrobial for a long time
Life leads to poultry prod fluo quinolone drug residual, destroys microecological balance etc..Therefore, clinical medicine, pharmacology, environment
It is required for establishing a kind of method of quick sensitive accurately detection Norfloxacin with food security etc., in clinical medicine, medicine
Of science, environment and food security etc. have very important significance.The Norfloxacin assay method master of document report at present
There are fluorimetry, spectrophotometry, high performance liquid chromatography and electrochemical methods etc., all there are sensitivity for these methods
Low, poor selectivity, time-consuming, need to use the shortcomings of special or complex instrument.
Electrochemical techniques have been used as a kind of high sensitivity, efficient and convenient, efficient tool for analyzing drug and human body
Important bioactive molecule in body fluid, various electrochemical sensors such as volt-ampere type, potentiometer-type, conductivity type, capacitive sensing
Device etc. has been widely used in the detection and analysis in terms of medicine, biology and environmental science.Molecularly imprinted polymer is a kind of tool
Have the material of artificial constructed recognition site, can preferentially other compounds and specifically bind target molecule, be a kind of simulation
The effective tool of natural biological receptor system such as antibody, hormone, enzyme.Molecularly imprinted polymer easily prepares, is at low cost and mechanical
Stability is good, improves trace analysis object measures in complex sample sensitivity, selectivity, accuracy and applicability.It is common
The method for preparing molecular engram sensor is that electrode surface synthesis imprinted polymer films, the party are really connected on by electrochemical polymerization
Method advantage is that film thickness is controllable, recognition site stable structure, fast response time.
Nano silver grain has unique optics, electricity, catalytic property, can be widely applied to catalyst material, battery electricity
Pole material, low temperature Heat Conduction Material and conductive material etc..Nano-particle is used as electrode active material, imparts electrode than tradition electricity
The more superior physical and chemical performance in pole can effectively improve the performances such as sensitivity and the selectivity of electrochemical sensor.
Invention content
The technical problem to be solved by the present invention is to provide a kind of norfloxacin molecular imprinted electrifications based on nanometer modified by silver
The preparation method for learning sensor and its application in selective enumeration method Norfloxacin.
It is of the invention to adopt the following technical scheme that solve above-mentioned technical problem, the Norfloxacin molecule based on nanometer modified by silver
The preparation method of trace electrochemical sensor, it is characterised in that detailed process is：Nano silver colloidal sol is uniformly applied to first
On the glass-carbon electrode of pretreatment, then using o-phenylenediamine as function monomer, Norfloxacin as template molecule, pass through electrochemistry
It is aggregated in and norfloxacin molecular imprinted o-phenylenediamine thin polymer film is obtained on the glass-carbon electrode of nanometer modified by silver, then from promise fluorine
Norfloxacin template molecule is removed in the o-phenylenediamine thin polymer film of husky star molecular engram and obtains the promise based on nanometer modified by silver
Flucloxacillin molecular imprinting electrochemical sensor.
Further preferably, the preparation side of the norfloxacin molecular imprinted electrochemical sensor based on nanometer modified by silver
Method, it is characterised in that the specific steps are：
（1）The nano silver colloidal sol of brand-new is evenly coated on the glass-carbon electrode of pretreatment, is received after drying at room temperature
The glass-carbon electrode of rice modified by silver；
（2）O-phenylenediamine and promise fluorine are added in HAc-NaAc buffer solutions of the molar concentration for 0.1mol/L, pH=3.5~5.0
Sha Xing, the molar concentration of o-phenylenediamine is 0.02mol/L in mixed solution, the ratio between molar concentration of Norfloxacin and o-phenylenediamine
It is 1:3~1:1；
（3）In step（2）Nitrogen 10min is continually fed into obtained mixed solution, by step（1）Obtained nanometer modified by silver
It is activated using square wave voltammetry in the sulfuric acid solution that glass-carbon electrode is 1mol/L in molar concentration, then repaiies the nano silver of activation
The glass-carbon electrode of decorations is inserted into mixed as working electrode, saturated calomel electrode as reference electrode and platinum plate electrode as auxiliary electrode
It closes in solution and forms three electrode body polymerization systems, glass carbon of the electrochemical polymerization in nano silver modified is carried out using cyclic voltammetry
Norfloxacin molecular imprinted o-phenylenediamine thin polymer film is obtained on electrode, operating condition is：Electric potential scanning range 0~
0.8V sweeps speed as 50mV/s, and the scanning number of turns is 5~20 circles；
（4）The trace electrode of nanometer modified by silver is put into the ammonium hydroxide that mass concentration is 1.5%, the potential of application -0.4V continues
Time 500s, for removing Norfloxacin from norfloxacin molecular imprinted o-phenylenediamine thin polymer film, then with secondary
Clear is washed to the norfloxacin molecular imprinted electrochemical sensor based on nanometer modified by silver.
It is of the present invention based on the norfloxacin molecular imprinted electrochemical sensor of nanometer modified by silver in selective enumeration method
Application in Norfloxacin, wherein linear detection range are 1*10-8mol·L-1~2.5*10-4mol·L-1, lowest detection is limited to
6.3*10-9mol·L-1, selectivity factor 8.3.
Compared with prior art, the beneficial effects of the invention are as follows：1st, the norfloxacin molecular imprinted electrification of nanometer modified by silver
Learning sensor has the linear detection range of non-constant width；2nd, the sensitivity of sensor is substantially increased, reduces detection limit；3rd, should
Electrochemical sensor high selectivity, strong antijamming capability；4th, the method for the present invention is simple, of low cost, easy to be fast to sample detection
It is prompt.
Specific embodiment
The above of the present invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to following embodiment, and all technologies realized based on the above of the present invention belong to this hair
Bright range.
Embodiment 1
（1）The nano silver colloidal sol of brand-new is evenly coated on the glass-carbon electrode of pretreatment, is received after drying at room temperature
The glass-carbon electrode of rice modified by silver；
（2）O-phenylenediamine and Norfloxacin are added in HAc-NaAc buffer solutions of the molar concentration for 0.1mol/L, pH=3.5,
It is 1 that the molar concentration of o-phenylenediamine, which is the ratio between 0.02mol/L, the molar concentration of Norfloxacin and o-phenylenediamine, in mixed solution:
2；
（3）In step（2）Nitrogen 10min is continually fed into obtained mixed solution, by step（1）Obtained nanometer modified by silver
It is activated using square wave voltammetry in the sulfuric acid solution that glass-carbon electrode is 1mol/L in molar concentration, then repaiies the nano silver of activation
The glass-carbon electrode of decorations is inserted into mixed as working electrode, saturated calomel electrode as reference electrode and platinum plate electrode as auxiliary electrode
It closes in solution and forms three electrode body polymerization systems, glass carbon of the electrochemical polymerization in nano silver modified is carried out using cyclic voltammetry
Norfloxacin molecular imprinted o-phenylenediamine thin polymer film is obtained on electrode, operating condition is：Electric potential scanning range 0~
0.8V sweeps speed as 50mV/s, and the scanning number of turns is 10 circles；
（4）The trace electrode of nanometer modified by silver is put into the ammonium hydroxide that mass concentration is 1.5%, the potential of application -0.4V continues
Time 500s, for removing Norfloxacin from norfloxacin molecular imprinted o-phenylenediamine thin polymer film, then with secondary
Clear is washed to the norfloxacin molecular imprinted electrochemical sensor based on nanometer modified by silver.
Embodiment 2
（1）The nano silver colloidal sol of brand-new is evenly coated on the glass-carbon electrode of pretreatment, is received after drying at room temperature
The glass-carbon electrode of rice modified by silver；
（2）O-phenylenediamine and Norfloxacin are added in HAc-NaAc buffer solutions of the molar concentration for 0.1mol/L, pH=4.0,
It is 1 that the molar concentration of o-phenylenediamine, which is the ratio between 0.02mol/L, the molar concentration of Norfloxacin and o-phenylenediamine, in mixed solution:
2；
（3）In step（2）Nitrogen 10min is continually fed into obtained mixed solution, by step（1）Obtained nanometer modified by silver
It is activated using square wave voltammetry in the sulfuric acid solution that glass-carbon electrode is 1mol/L in molar concentration, then repaiies the nano silver of activation
The glass-carbon electrode of decorations is inserted into mixed as working electrode, saturated calomel electrode as reference electrode and platinum plate electrode as auxiliary electrode
It closes in solution and forms three electrode body polymerization systems, glass carbon of the electrochemical polymerization in nano silver modified is carried out using cyclic voltammetry
Norfloxacin molecular imprinted o-phenylenediamine thin polymer film is obtained on electrode, operating condition is：Electric potential scanning range 0~
0.8V sweeps speed as 50mV/s, and the scanning number of turns is 10 circles；
（4）The trace electrode of nanometer modified by silver is put into the ammonium hydroxide that mass concentration is 1.5%, the potential of application -0.4V continues
Time 500s, for removing Norfloxacin from norfloxacin molecular imprinted o-phenylenediamine thin polymer film, then with secondary
Clear is washed to the norfloxacin molecular imprinted electrochemical sensor based on nanometer modified by silver.
The norfloxacin molecular imprinted electrochemical sensor based on nanometer modified by silver is for selectivity made from the present embodiment
During detecting Norfloxacin：Linear detection range is 1*10-8mol·L-1~2.5*10-4mol·L-1, lowest detection is limited to
6.3*10-9mol·L-1, selectivity factor（Nanometer modified by silver trace electrode becomes the opposite peak current of Norfloxacin sample response
The ratio that the opposite peak current that change amount is generated with the interfering substance to same concentrations similar structures changes）It is 8.3.
Embodiment 3
（1）The nano silver colloidal sol of brand-new is evenly coated on the glass-carbon electrode of pretreatment, is received after drying at room temperature
The glass-carbon electrode of rice modified by silver；
（2）O-phenylenediamine and Norfloxacin are added in HAc-NaAc buffer solutions of the molar concentration for 0.1mol/L, pH=4.0,
It is 1 that the molar concentration of o-phenylenediamine, which is the ratio between 0.02mol/L, the molar concentration of Norfloxacin and o-phenylenediamine, in mixed solution:
1；
（3）In step（2）Nitrogen 10min is continually fed into obtained mixed solution, by step（1）Obtained nanometer modified by silver
It is activated using square wave voltammetry in the sulfuric acid solution that glass-carbon electrode is 1mol/L in molar concentration, then repaiies the nano silver of activation
The glass-carbon electrode of decorations is inserted into mixed as working electrode, saturated calomel electrode as reference electrode and platinum plate electrode as auxiliary electrode
It closes in solution and forms three electrode body polymerization systems, glass carbon of the electrochemical polymerization in nano silver modified is carried out using cyclic voltammetry
Norfloxacin molecular imprinted o-phenylenediamine thin polymer film is obtained on electrode, operating condition is：Electric potential scanning range 0~
0.8V sweeps speed as 50mV/s, and the scanning number of turns is 10 circles；
（4）The trace electrode of nanometer modified by silver is put into the ammonium hydroxide that mass concentration is 1.5%, the potential of application -0.4V continues
Time 500s, for removing Norfloxacin from norfloxacin molecular imprinted o-phenylenediamine thin polymer film, then with secondary
Clear is washed to the norfloxacin molecular imprinted electrochemical sensor based on nanometer modified by silver.
Embodiment 4
（1）The nano silver colloidal sol of brand-new is evenly coated on the glass-carbon electrode of pretreatment, is received after drying at room temperature
The glass-carbon electrode of rice modified by silver；
（2）O-phenylenediamine and Norfloxacin are added in HAc-NaAc buffer solutions of the molar concentration for 0.1mol/L, pH=5.0,
It is 1 that the molar concentration of o-phenylenediamine, which is the ratio between 0.02mol/L, the molar concentration of Norfloxacin and o-phenylenediamine, in mixed solution:
3；
（3）In step（2）Nitrogen 10min is continually fed into obtained mixed solution, by step（1）Obtained nanometer modified by silver
It is activated using square wave voltammetry in the sulfuric acid solution that glass-carbon electrode is 1mol/L in molar concentration, then repaiies the nano silver of activation
The glass-carbon electrode of decorations is inserted into mixed as working electrode, saturated calomel electrode as reference electrode and platinum plate electrode as auxiliary electrode
It closes in solution and forms three electrode body polymerization systems, glass carbon of the electrochemical polymerization in nano silver modified is carried out using cyclic voltammetry
Norfloxacin molecular imprinted o-phenylenediamine thin polymer film is obtained on electrode, operating condition is：Electric potential scanning range 0~
0.8V sweeps speed as 50mV/s, and the scanning number of turns is 20 circles；
（4）The trace electrode of nanometer modified by silver is put into the ammonium hydroxide that mass concentration is 1.5%, the potential of application -0.4V continues
Time 500s, for removing Norfloxacin from norfloxacin molecular imprinted o-phenylenediamine thin polymer film, then with secondary
Clear is washed to the norfloxacin molecular imprinted electrochemical sensor based on nanometer modified by silver.
Basic principle, main features and advantages embodiment above describes the present invention, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe the originals of the present invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (4)
1. the preparation method of the norfloxacin molecular imprinted electrochemical sensor based on nanometer modified by silver, it is characterised in that specific mistake
Cheng Wei：Nano silver colloidal sol is uniformly applied on the glass-carbon electrode of pretreatment first, then using o-phenylenediamine as function list
Body, Norfloxacin obtain Norfloxacin point by electrochemical polymerization as template molecule on the glass-carbon electrode of nanometer modified by silver
The o-phenylenediamine thin polymer film of sub- trace, then promise fluorine is removed from norfloxacin molecular imprinted o-phenylenediamine thin polymer film
Husky star template molecule obtains the norfloxacin molecular imprinted electrochemical sensor based on nanometer modified by silver.
2. the preparation side of the norfloxacin molecular imprinted electrochemical sensor according to claim 1 based on nanometer modified by silver
Method, it is characterised in that the specific steps are：
（1）The nano silver colloidal sol of brand-new is evenly coated on the glass-carbon electrode of pretreatment, is received after drying at room temperature
The glass-carbon electrode of rice modified by silver；
（2）O-phenylenediamine and promise fluorine are added in HAc-NaAc buffer solutions of the molar concentration for 0.1mol/L, pH=3.5~5.0
Sha Xing, the molar concentration of o-phenylenediamine is 0.02mol/L in mixed solution, the ratio between molar concentration of Norfloxacin and o-phenylenediamine
It is 1:3~1:1；
（3）In step（2）Nitrogen 10min is continually fed into obtained mixed solution, by step（1）Obtained nanometer modified by silver
It is activated using square wave voltammetry in the sulfuric acid solution that glass-carbon electrode is 1mol/L in molar concentration, then repaiies the nano silver of activation
The glass-carbon electrode of decorations is inserted into mixed as working electrode, saturated calomel electrode as reference electrode and platinum plate electrode as auxiliary electrode
It closes in solution and forms three electrode body polymerization systems, glass carbon of the electrochemical polymerization in nano silver modified is carried out using cyclic voltammetry
Norfloxacin molecular imprinted o-phenylenediamine thin polymer film is obtained on electrode, operating condition is：Electric potential scanning range 0~
0.8V sweeps speed as 50mV/s, and the scanning number of turns is 5~20 circles；
（4）The trace electrode of nanometer modified by silver is put into the ammonium hydroxide that mass concentration is 1.5%, the potential of application -0.4V continues
Time 500s, for removing Norfloxacin from norfloxacin molecular imprinted o-phenylenediamine thin polymer film, then with secondary
Clear is washed to the norfloxacin molecular imprinted electrochemical sensor based on nanometer modified by silver.
3. the method as claimed in claim 1 or 2 norfloxacin molecular imprinted electrochemistry obtained based on nanometer modified by silver passes
Application of the sensor in selective enumeration method Norfloxacin.
4. it is according to claim 3 based on the norfloxacin molecular imprinted electrochemical sensor of nanometer modified by silver in selectivity
Detect the application in Norfloxacin, it is characterised in that：Linear detection range is 1*10-8mol·L-1~2.5*10-4mol·L-1,
Lowest detection is limited to 6.3*10-9mol·L-1, selectivity factor 8.3.
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Cited By (2)
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| CN109270135A (en) * | 2018-11-19 | 2019-01-25 | 肇庆市华师大光电产业研究院 | A kind of modified electrode and preparation method thereof for norfloxacin molecular imprinted electrochemical sensor |
| CN112114019A (en) * | 2020-08-10 | 2020-12-22 | 中国科学院烟台海岸带研究所 | Potentiometric antifouling sensor based on indole active substance release and application thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109270135A (en) * | 2018-11-19 | 2019-01-25 | 肇庆市华师大光电产业研究院 | A kind of modified electrode and preparation method thereof for norfloxacin molecular imprinted electrochemical sensor |
| CN112114019A (en) * | 2020-08-10 | 2020-12-22 | 中国科学院烟台海岸带研究所 | Potentiometric antifouling sensor based on indole active substance release and application thereof |
| CN112114019B (en) * | 2020-08-10 | 2022-11-29 | 中国科学院烟台海岸带研究所 | Potentiometric antifouling sensor based on indole active substance release and application thereof |
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