CN105699470A - Magnetic molecular imprinting electrochemical sensor for detecting trace sulfadimidine - Google Patents
Magnetic molecular imprinting electrochemical sensor for detecting trace sulfadimidine Download PDFInfo
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- CN105699470A CN105699470A CN201610195286.2A CN201610195286A CN105699470A CN 105699470 A CN105699470 A CN 105699470A CN 201610195286 A CN201610195286 A CN 201610195286A CN 105699470 A CN105699470 A CN 105699470A
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- 229960002135 sulfadimidine Drugs 0.000 title claims abstract description 39
- ASWVTGNCAZCNNR-UHFFFAOYSA-N sulfamethazine Chemical compound CC1=CC(C)=NC(NS(=O)(=O)C=2C=CC(N)=CC=2)=N1 ASWVTGNCAZCNNR-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 21
- 230000008569 process Effects 0.000 claims description 10
- 238000002484 cyclic voltammetry Methods 0.000 claims description 9
- 239000012530 fluid Substances 0.000 claims description 7
- 229920000642 polymer Polymers 0.000 claims description 7
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 6
- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229910019142 PO4 Inorganic materials 0.000 claims description 5
- 239000008366 buffered solution Substances 0.000 claims description 5
- 239000003480 eluent Substances 0.000 claims description 5
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 5
- 239000010452 phosphate Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 4
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 4
- 239000012498 ultrapure water Substances 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000001548 drop coating Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- DZGCGKFAPXFTNM-UHFFFAOYSA-N ethanol;hydron;chloride Chemical compound Cl.CCO DZGCGKFAPXFTNM-UHFFFAOYSA-N 0.000 claims description 3
- 238000012986 modification Methods 0.000 claims description 3
- 230000004048 modification Effects 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 3
- 235000011149 sulphuric acid Nutrition 0.000 claims description 3
- 239000001117 sulphuric acid Substances 0.000 claims description 3
- 230000002000 scavenging effect Effects 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 13
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 abstract description 4
- 230000035945 sensitivity Effects 0.000 abstract description 4
- TURHTASYUMWZCC-UHFFFAOYSA-N Olaquindox [BAN:INN] Chemical compound C1=CC=C2N([O-])C(C)=C(C(=O)NCCO)[N+](=O)C2=C1 TURHTASYUMWZCC-UHFFFAOYSA-N 0.000 abstract description 2
- 229960003638 dopamine Drugs 0.000 abstract description 2
- 229950010210 olaquindox Drugs 0.000 abstract description 2
- 238000006116 polymerization reaction Methods 0.000 abstract description 2
- 230000000630 rising effect Effects 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 5
- 238000001903 differential pulse voltammetry Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 239000008267 milk Substances 0.000 description 3
- 235000013336 milk Nutrition 0.000 description 3
- 210000004080 milk Anatomy 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001819 mass spectrum Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- -1 potassium ferricyanide Chemical compound 0.000 description 2
- 229940124530 sulfonamide Drugs 0.000 description 2
- 238000007445 Chromatographic isolation Methods 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 102000001554 Hemoglobins Human genes 0.000 description 1
- 108010054147 Hemoglobins Proteins 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 235000013601 eggs Nutrition 0.000 description 1
- 238000001962 electrophoresis Methods 0.000 description 1
- 125000000031 ethylamino group Chemical group [H]C([H])([H])C([H])([H])N([H])[*] 0.000 description 1
- 229910021397 glassy carbon Inorganic materials 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 210000000987 immune system Anatomy 0.000 description 1
- 238000003018 immunoassay Methods 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 230000005426 magnetic field effect Effects 0.000 description 1
- 238000007885 magnetic separation Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229920000344 molecularly imprinted polymer Polymers 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002858 neurotransmitter agent Substances 0.000 description 1
- 238000002414 normal-phase solid-phase extraction Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 244000144977 poultry Species 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- VACCAVUAMIDAGB-UHFFFAOYSA-N sulfamethizole Chemical compound S1C(C)=NN=C1NS(=O)(=O)C1=CC=C(N)C=C1 VACCAVUAMIDAGB-UHFFFAOYSA-N 0.000 description 1
- FDDDEECHVMSUSB-UHFFFAOYSA-N sulfanilamide Chemical compound NC1=CC=C(S(N)(=O)=O)C=C1 FDDDEECHVMSUSB-UHFFFAOYSA-N 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004809 thin layer chromatography Methods 0.000 description 1
- 230000002485 urinary effect Effects 0.000 description 1
Classifications
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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
- G01N27/416—Systems
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Biological Materials (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
- Polyoxymethylene Polymers And Polymers With Carbon-To-Carbon Bonds (AREA)
Abstract
The invention relates to a magnetic molecular imprinting electrochemical sensor for detecting trace sulfadimidine. The magnetic molecular imprinting electrochemical sensor of sulfadimidine is prepared by adopting a magnetic reduced graphene modified magnetic electrode and applying dopamine to carry out self-polymerization. When the concentration of olaquindox is in a range of 10.0nM-200.0nM, an electrochemical signal rising degree has a good linear relation with the concentration of sulfadimidine; and the detection limit of a method reaches 0.1nM. When the sensor is used for detecting an actual sample, the yield reaches 92.6%-101.7%; and with the adoption of the magnetic molecular imprinting electrochemical sensor, the sensitivity and selectivity of sulfadimidine are improved, and the automation of detection of trace sulfadimidine is easy to realize.
Description
Technical field
The invention belongs to new function material, electrochemical sensing detection technique field, relate to a kind of magnetic molecularly imprinted electrochemical sensor, particularly a kind of magnetic molecularly imprinted electrochemical sensor for detecting trace sulfadimidine。
Background technology
Sulfadimidine (Sulfadimidine, SM2), has another name called sulfadimidine, Urolucosil, and systematic naming method is N-(4,6-dimethyl-2-pyrimidine radicals)-4-aminobenzenesul fonamide。Sulfadimidine, sulfa drugs is a class broad-spectrum antiseptic medicine, is widely used in prevention and the treatment of animal class particularly livestock and poultry。But what human body was excessive takes in sulfadimidine affects immune system and the urinary system of human body, destroys body normal flora ecological balance, pathogenic bacterium are caused to produce drug resistance。Therefore the detection of sulfadimidine is controlled particularly important。At present the conventional detection method of sulfa drugs being had: using high performance liquid chromatography tandem mass spectrum method, gold immune analysis method, high performance liquid chromatography, chemiluminescence analysis method, thin layer chromatography, capillary superintends and directs electrophoresis etc.。But these methods are typically necessary the pre-treatment carrying out complex sample, and using high performance liquid chromatography tandem mass spectrum method combines the high separating power of chromatograph and mass spectrographic high qualitative ability, but instrument ability is more expensive, the laboratory technician using instrument also there is higher operation requirement。The advantages such as immunoassay has sensitive, economic, quick, but this methods experiment gets up more complicated。
It is very important for strictly controlling the residual amount of sulfanilamide in meat, milk and eggs, and therefore a kind of detection method that quickly effectively can reuse is particularly important。Molecular imprinting (MIT) is a kind of new technique with structure effect pre-setting, specially identity and broad applicability in recent years risen。The molecularly imprinted polymer prepared based on this technology has affinity and selectivity height, and anti-adverse environment ability is strong, good stability, long service life, being widely used ground feature, molecular imprinting is in chromatographic isolation, and Solid-Phase Extraction, bionical sensing are all formed and be widely applied。In conjunction with the magnetic blotting polymer that magnetic separation technique and molecular imprinting synthesize, can Selective recognition target molecule, again can sharp separation under outside magnetic field effect, therefore become study hotspot in recent years。Dopamine is neurotransmitter, containing abundant catechol and ethylamino active function groups, has good biocompatibility and oxidation polymerization ability, almost can adhere on any matrix。In recent years, it is widely used in the immobilization of the biological substances such as antibody, enzyme and hemoglobin, is a kind of good biological fixation material and molecular engram monomer。
Magnetic molecularly imprinted technology is combined with sensor, it is possible to obtain high sensitivity, high selective biosensor, had relevant report at present, but the detection being applied to trace sulfadimidine does not have correlational study temporarily。
Summary of the invention
For solving the deficiencies in the prior art, a kind of magnetic molecularly imprinted electrochemical sensor for trace sulfadimidine of offer is provided, can high sensitivity, highly selective be used for detecting trace sulfadimidine。
A kind of magnetic molecularly imprinted electrochemical sensor for detecting trace sulfadimidine of the present invention, it is characterised in that described magnetic molecularly imprinted electrochemical sensor is prepared by the following method:
(1) process of magnetic core electrode:
Magnetic core glass-carbon electrode is put in the sulphuric acid of 0.2M and activates after 20min, carry out surface finish process with the alpha-alumina powder of 1.0,0.3 and 0.05 μm successively, with ultrapure water totally after dry, then electrode is placed in the K of 5mM3[Fe(CN)6] in solution, in-0.2V～0.6V potential range, it is circulated volt-ampere (CV) scanning until obtaining stable cyclic voltammogram with the speed of 100mV/s。
(2) modification of magnetic core electrode:
Weigh 10mg magnetizing reduction Graphene (Fe3O4RGO) it is placed in 4mL water ultrasonic disperse 10min, forms dispersion liquid。Pipette the 5 μ careful drop coatings of L dispersion liquid in electrode surface with micropipette rifle, be placed under infrared lamp drying for standby。
(3) preparation of molecular engram polymer fluid:
Sulfadimidine is dissolved in the sulfadimidine solution being configured to 5mM in N, N-dimethyl pyrimidine, and dopamine hydrochloride is dissolved in water and is configured to 10mM dopamine hydrochloride solution；Pipetting each 0.1mL of above-mentioned solution respectively, utilize phosphate buffered solution to regulate pH value, after supersound process 20min, solution becomes faint yellow stand-by；
(4) structure of sensor:
Magnetic core electrode after modifying is immersed in polymer fluid, adopt cyclic voltammetry to scan a fixing turn under the speed of 100mV/S under-0.2V～0.6V, it is placed in 0.2M hydrochloric acid-ethanol (1:2, V/V) eluent to clean, obtains the magnetic molecularly imprinted electrochemical sensor of sulfadimidine。
Further feature according to molecular imprinting electrochemical sensor of the present invention, in described step (3), it is 7.5 that phosphate buffered solution regulates pH value。
Further feature according to molecular imprinting electrochemical sensor of the present invention, in described step (4), the scanning number of turns is 20 circles。
Further feature according to molecular imprinting electrochemical sensor of the present invention, in described step (4), eluent scavenging period is 20min。
Magnetic molecularly imprinted electrochemical sensor for detecting trace sulfadimidine of the present invention overcomes prior art, and when detecting trace sulfadimidine, to there is method excessively loaded down with trivial details, the shortcomings such as step is complicated, improve sensitivity and the selectivity of detection better, the detection for trace sulfadimidine is prone to automatization。
Accompanying drawing explanation
Fig. 1 is that different modifying electrode is at K3[Fe(CN)6] cyclic voltammetry curve in solution, in figure, a: naked magnetic core electrode；B:Fe3O4RGO/ magnetic core electrode；C:MIP modified electrode；D: the MIP modified electrode after eluted template。
Fig. 2 a is the scanning electron microscope diagram of MIP modified electrode, and Fig. 2 b is the scanning electron microscope diagram of the MIP modified electrode after eluting。
Fig. 3 is standard absorption curve of the present invention。
Detailed description of the invention
Embodiment 1: the structure of the magnetic molecularly imprinted electrochemical sensor for detecting trace sulfadimidine of the present invention, it is characterised in that described magnetic molecularly imprinted electrochemical sensor is prepared by the following method:
(1) process of magnetic core electrode:
Magnetic core glass-carbon electrode is put in the sulphuric acid of 0.2M and activates after 20min, carry out surface finish process with the alpha-alumina powder of 1.0,0.3 and 0.05 μm successively, with ultrapure water totally after dry, then electrode is placed in the K of 5mM3[Fe(CN)6] in solution, in-0.2V～0.6V potential range, it is circulated volt-ampere (CV) scanning until obtaining stable cyclic voltammogram with the speed of 100mV/s。
(2) modification of magnetic core electrode:
Weigh 10mg magnetizing reduction Graphene Fe3O4RGO is placed in 4mL water ultrasonic disperse 10min, forms dispersion liquid。Pipette the 5 μ careful drop coatings of L dispersion liquid in electrode surface with micropipette rifle, be placed under infrared lamp drying for standby。
(3) preparation of molecular engram polymer fluid:
Sulfadimidine is dissolved in the sulfadimidine solution being configured to 5mM in N, N-dimethyl pyrimidine, and dopamine hydrochloride is dissolved in water and is configured to 10mM dopamine hydrochloride solution；Pipetting each 0.1mL of above-mentioned solution respectively, utilize phosphate buffered solution to regulate pH value, after supersound process 20min, solution becomes faint yellow stand-by；
(4) structure of sensor:
Magnetic core electrode after modifying is immersed in polymer fluid, adopt cyclic voltammetry to scan a fixing turn under the speed of 100mV/S under-0.2V～0.6V, the eluent being placed in 0.2M hydrochloric acid-ethanol (1:2, V/V) cleans, and obtains the magnetic molecularly imprinted electrochemical sensor of sulfadimidine。
Embodiment 2: the cyclic voltammetric of the magnetic molecularly imprinted electrochemical sensor for detecting trace sulfadimidine of the present invention characterizes
Owing to the trace hole in film as the passage of electron transmission, can use K3[Fe(CN)6] for probe, characterize the surface nature of various electrodes according to the size of its electric current。As it is shown in figure 1, Different electrodes is at the K of 5mM3[Fe(CN)6] cyclic voltammogram significant difference in solution。Curve a is the cyclic voltammogram of naked magnetic core electrode, and oxidoreduction peak is obvious。Shown in curve b, when at one layer of Fe of magnetic glassy carbon electrode finishing3O4After rGO complex, peak current has increase clearly, and this is due to Fe3O4RGO composite conductivity is fine, can promote the electron transmission of electrode surface, increases current signal。Shown in curve c, when after the electrode surface electropolymerization blotting membrane after modifying, it is possible to finding that oxidoreduction peak current is decreased obviously, because after electropolymerization MIPs, the electron transfer process of sensor is hindered。As shown in curve d, template molecule sulfadimidine is eluted, and has hole to allow electronics transmit, and signal recovers。
Embodiment 3: the scanning electron microscope of the different modifying electrode of the magnetic molecularly imprinted electrochemical sensing for detecting trace sulfadimidine of the present invention characterizes
Adopt scanning electron microscope, the microstructure of different modifying electrode has been characterized。As shown in Figure 2 a, molecular engram film rear electrode smooth surface on electrode face finish, illustrate that imprinting effect is good；After eluting, owing to template molecule is eluted, therefore leaving many holes on this molecular engram film surface, therefore surface becomes coarse (referring to Fig. 2 b)。
Embodiment 4: the range of linearity and detection limit experiment
With optimal conditions, by trace electrode in K3Fe(CN)6Solution carries out differential pulse voltammetry scanning, measures oxidation peak current and be designated as I0Then being immersed in the olaquindox solution of variable concentrations by trace electrode the Adsorption Phase time together, the oxidation peak current recorded after absorption is designated as I, experiment Relative Peak electric current △ I (△ I=I0-I) curent change is described。As it is shown on figure 3, in the concentration range that concentration is 10-200nM, △ I (μ A) and sulfadimidine concentration C (nM) present good linear relationship, and its equation of linear regression is △ I=0.872.9C+48.51, R2=0.9918, detection is limited to 0.1Nm。
Embodiment 5: repeatability and stability experiment
The repeatability of molecular imprinting electrochemical sensor is by carrying out DPV detection in the same molecular engram electrode of the preparation sulfadimidine solution to 100nM under mensuration the same terms, relative standard deviation is 4.05%, it was shown that trace electrode has good reversibility and repeatability。
The stability of sensor is also the key factor that whether good research sensor is, prepares 3 identical sensors under the same conditions, is put in refrigerator and preserves 2 weeks, carries out DPV detection afterwards respectively in the sulfadimidine solution to 100nM。End product finds after showing two weeks that response current value is original 89%, it was shown that sensor has good stability。
Embodiment 6: actual sample measures
Take centrifugal 10min under milk 2mL, 3000rpm to be measured, abandon butterfat, ultra-pure water dilutes, after putting into trace electrode 10min, marking electrode is transferred in potassium ferricyanide test fluid, measures potassium ferricyanide probe molecule current-responsive on trace electrode with differential pulse voltammetry。Then adopting standard addition method to detect after being added thereto to a certain amount of sulfadimidine, measurement result is in Table 1。The response rate of method is 95.9%-103.2% as shown in Table 1, and relative standard deviation is 1.67%-3.28%。
Table 1 milk sample analysis
| Sequence number | Add scalar nM | Actually detected nM | The response rate (%) | RSD (%) |
| 1 | 10 | 9.75 | 97.5 | 2.73 |
| 2 | 20 | 20.63 | 103.2 | 3.28 |
| 3 | 30 | 28.78 | 95.9 | 1.67 |
| 4 | 50 | 48.42 | 96.8 | 3.25 |
| 5 | 70 | 71.23 | 101.7 | 2.29 |
Claims (4)
1. the magnetic molecularly imprinted electrochemical sensor being used for detecting trace sulfadimidine, it is characterised in that described magnetic molecularly imprinted electrochemical sensor is prepared by the following method:
(1) process of magnetic core electrode:
Magnetic core glass-carbon electrode is put in the sulphuric acid of 0.2M and activates after 20min, carry out surface finish process with the alpha-alumina powder of 1.0,0.3 and 0.05 μm successively, with ultrapure water totally after dry, then electrode is placed in the K of 5mM3[Fe(CN)6] in solution, in-0.2V～0.6V potential range, it is circulated volt-ampere (CV) scanning until obtaining stable cyclic voltammogram with the speed of 100mV/s；
(2) modification of magnetic core electrode:
Weigh 10mg magnetizing reduction Graphene Fe3O4RGO, is placed in 4mL water ultrasonic disperse 10min, forms dispersion liquid；Pipette the 5 μ careful drop coatings of L dispersion liquid in electrode surface with micropipette rifle, be placed under infrared lamp drying for standby；
(3) preparation of molecular engram polymer fluid:
Sulfadimidine is dissolved in the sulfadimidine solution being configured to 5mM in N, N-dimethyl pyrimidine, dopamine hydrochloride is dissolved in water and is configured to 10mM dopamine hydrochloride solution；Pipetting each 0.1mL of above-mentioned solution respectively, utilize phosphate buffered solution to regulate pH value, after supersound process 20min, solution becomes faint yellow stand-by；
(4) structure of sensor:
Magnetic core electrode after modifying is immersed in polymer fluid, adopt cyclic voltammetry to scan a fixing turn under the speed of 100mV/S under-0.2V～0.6V, it is placed in 0.2M hydrochloric acid-ethanol (1:2, V/V) eluent to clean, obtains the magnetic molecularly imprinted electrochemical sensor of sulfadimidine。
2. magnetic molecularly imprinted electrochemical sensor according to claim 1, it is characterised in that: in described step (3), it is 7.5 that phosphate buffered solution regulates pH value。
3. magnetic molecularly imprinted electrochemical sensor according to claim 1, it is characterised in that: in described step (4), the scanning number of turns is 20 circles。
4. magnetic molecularly imprinted electrochemical sensor according to claim 1, it is characterised in that: in described step (4), eluent scavenging period is 20min。
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105891290A (en) * | 2016-04-01 | 2016-08-24 | 肇庆学院 | Magnetic molecular imprinting electrochemical sensor used for detecting trace sulfadimidine |
| CN106018533A (en) * | 2016-07-01 | 2016-10-12 | 肇庆学院 | Molecularly imprinted electrochemical sensor for detecting trace sulfamonomethoxine |
| CN106053565A (en) * | 2016-06-27 | 2016-10-26 | 肇庆学院 | Electrochemical sensor for detecting trace olaquindox |
| CN108387632A (en) * | 2018-02-24 | 2018-08-10 | 云南大学 | A kind of Eu3+Selective quantitative detecting method |
| CN110567903A (en) * | 2019-08-08 | 2019-12-13 | 安徽师范大学 | Ferroferric oxide modified graphite paper-based molecular imprinting sensor and preparation method and application thereof |
| CN112114011A (en) * | 2020-09-13 | 2020-12-22 | 山西大学 | Magnetic control high-flux electrochemical sensor and preparation method and application thereof |
| CN113899795A (en) * | 2021-09-23 | 2022-01-07 | 中国水产科学研究院黄海水产研究所 | Electrochemical sensor based on molecular imprinting, preparation method and sulfadimidine detection method |
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| CN103801269A (en) * | 2012-11-14 | 2014-05-21 | 江南大学 | Preparation of surface imprinting graphene composite material |
| CN104181217A (en) * | 2014-04-29 | 2014-12-03 | 南昌大学 | Construction and application of impedance type electrochemical sensor based on molecularly imprinted polymer with magnetic surface |
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| A. GUZMAN-VAZQUEZ DE PRADA ET.AL.: "A method for the quantification of low concentration sulfamethazine residues in milk based on molecularly imprinted clean-up and surface preconcentration at a Nafion-modified glassy carbon electrode", 《JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS》 * |
| QING HAN ET.AL.: "Fe3O4@rGO doped molecularly imprinted polymer membrane based on magnetic field directed self-assembly for the determination of amaranth", 《TALANTA》 * |
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| CN106018533A (en) * | 2016-07-01 | 2016-10-12 | 肇庆学院 | Molecularly imprinted electrochemical sensor for detecting trace sulfamonomethoxine |
| CN108387632A (en) * | 2018-02-24 | 2018-08-10 | 云南大学 | A kind of Eu3+Selective quantitative detecting method |
| CN110567903A (en) * | 2019-08-08 | 2019-12-13 | 安徽师范大学 | Ferroferric oxide modified graphite paper-based molecular imprinting sensor and preparation method and application thereof |
| CN110567903B (en) * | 2019-08-08 | 2022-03-15 | 安徽师范大学 | Ferroferric oxide modified graphite paper-based molecular imprinting sensor and preparation method and application thereof |
| CN112114011A (en) * | 2020-09-13 | 2020-12-22 | 山西大学 | Magnetic control high-flux electrochemical sensor and preparation method and application thereof |
| CN113899795A (en) * | 2021-09-23 | 2022-01-07 | 中国水产科学研究院黄海水产研究所 | Electrochemical sensor based on molecular imprinting, preparation method and sulfadimidine detection method |
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