CN105891290A - Magnetic molecular imprinting electrochemical sensor used for detecting trace sulfadimidine - Google Patents
Magnetic molecular imprinting electrochemical sensor used for detecting trace sulfadimidine Download PDFInfo
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- CN105891290A CN105891290A CN201610206836.6A CN201610206836A CN105891290A CN 105891290 A CN105891290 A CN 105891290A CN 201610206836 A CN201610206836 A CN 201610206836A CN 105891290 A CN105891290 A CN 105891290A
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Abstract
The invention relates to a magnetic molecular imprinting electrochemical sensor used for detecting trace sulfadimidine. A magnetic electrode modified by magnetic reduction graphene, dopamine auto-agglutination is adopted, and the sulfadimidine magnetic molecular imprinting electrochemical sensor is prepared. When the concentration of olaquindox is within the range of 10.0 nM-200.0 nM, the rise degree of electrochemical signals has a good linear relation with the concentration of sulfadimidine, and a method detection limit reaches 0.1 nM. The sensor is used for detecting actual samples, and the recovery rate reaches 92.6-101.7%. The sensor improves sensitivity and selectivity of sulfadimidine, and detection of trace sulfadimidine is easy to automate.
Description
Technical field
The invention belongs to new function material, electrochemical sensing detection technique field, relate to a kind of magnetic molecule print
Mark electrochemical sensor, a kind of magnetic molecularly imprinted electrochemistry for detecting trace sulfadimidine
Sensor.
Background technology
Sulfadimidine (Sulfadimidine, SM2), has another name called sulfadimidine, Urolucosil, system
Named N-(4,6-dimethyl-2-pyrimidine radicals)-4-aminobenzene sulfonamide.Sulfadimidine, sulfa drugs is
One class broad-spectrum antiseptic medicine, is widely used in prevention and the treatment of animal class particularly livestock and poultry.But human body
The sulfadimidine of taking in of excess affects immune system and the urinary system of human body, destroys body normal bacteria all living creatures
State balances, and causes pathogenic bacteria to produce drug resistance.Therefore the detection to sulfadimidine controls particularly important.Mesh
The front detection method commonly using sulfa drugs has: high performance liquid chromatography tandem mass spectrum method, gold immunoassay side
Method, high performance liquid chromatography, chemiluminescence analysis method, thin-layered chromatography, capillary superintends and directs electrophoresis etc..But these
Method is typically necessary the pre-treatment carrying out complex sample, and high performance liquid chromatography tandem mass spectrum method is comprehensive
The high separating power of chromatogram and mass spectrographic high qualitative ability, but instrument ability is more expensive, to using instrument
Laboratory technician also has higher operation requirement.The advantages such as immunoassay has sensitive, economic, quick, but this
Plant methods experiment and get up more complicated.
It is very important for strictly controlling the residual amount of sulfanilamide in meat, milk and eggs, and therefore one quickly has
The detection method that effect can reuse is particularly important.Molecular imprinting (MIT) is a kind of tool in recent years risen
There is the new technology of structure effect pre-setting, specially identity and broad applicability.The molecular engram prepared based on this technology
Polymer has compatibility and selective height, and anti-adverse environment ability is strong, good stability, and service life is long, should
By feature widely, molecular imprinting is in chromatographic isolation, and SPE, bionical sensing are all formed widely should
With.The magnetic blotting polymer synthesized in conjunction with magnetic separation technique and molecular imprinting, can Selective recognition
Target molecule, again can quick separating under outside magnetic field effect, therefore become study hotspot in recent years.Dopamine
Neurotransmitter, containing abundant catechol and ethylamino active function groups, have good biocompatibility and
Oxidation polymerization ability, almost can adhere on any matrix.In recent years, antibody, enzyme and blood red egg it are widely used in
The white immobilization waiting biological substance, 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 biology
Sensor, has had relevant report, but the detection being applied to trace sulfadimidine has not had relevant temporarily
Research.
Summary of the invention
For solving the deficiencies in the prior art, the invention reside in a kind of magnetic for trace sulfadimidine of offer
Molecular imprinting electrochemical sensor, can high sensitivity, highly selective be used for detecting trace sulfadimidine.
A kind of magnetic molecularly imprinted electrochemical sensing for detecting trace sulfadimidine of the present invention
Device, it is characterised in that described magnetic molecularly imprinted electrochemical sensor is prepared by the following method:
(1) process of magnetic core electrode:
After magnetic core glass-carbon electrode is put in the sulfuric acid of 0.2M activation 20min, successively by 1.0,0.3 and 0.05 μm
Alpha-alumina powder carry out surface finish process, with ultrapure water clean after dry, then electrode is placed in
The K of 5mM3[Fe(CN)6] in solution, in-0.2V～0.6V potential range, the speed with 100mV/s is carried out
Cyclic voltammetric (CV) scanning is until obtaining stable cyclic voltammogram.
(2) modification of magnetic core electrode:
Weigh 10mg magnetizing reduction Graphene (Fe3O4@rGO) it is placed in ultrasonic disperse 10min in 4mL water,
Form dispersion liquid.Pipette the 5 μ careful drop coatings of L dispersion liquid in electrode surface with micropipette rifle, be placed in infrared lamp
Lower drying for standby.
(3) preparation of molecular engram polymer fluid:
Sulfadimidine is dissolved in that to be configured to the sulfadimidine of 5mM in N, N-dimethyl pyrimidine molten
Liquid, Dopamine hydrochloride is dissolved in water and is configured to 10mM Dopamine hydrochloride solution；Pipette above-mentioned solution respectively each
0.1mL, utilizes PBS to regulate pH value, and after ultrasonically treated 20min, solution becomes faint yellow
Stand-by；
(4) structure of sensor:
Magnetic core electrode after modifying immerses in polymer fluid, uses cyclic voltammetry with 100 under-0.2V～0.6V
Scan a fixing turn under the speed of mV/S, be placed in 0.2M hydrochloric acid-ethanol (1:2, V/V) eluent and clean,
Obtain the magnetic molecularly imprinted electrochemical sensor of sulfadimidine.
According to the further feature of molecular imprinting electrochemical sensor of the present invention, in described step (3),
PBS regulation pH value is 7.5.
According to the further feature of molecular imprinting electrochemical sensor of the present invention, in described step (4),
The scanning number of turns is 20 circles.
According to the further feature of molecular imprinting electrochemical sensor of the present invention, in described step (4),
Eluent scavenging period is 20min.
Magnetic molecularly imprinted electrochemical sensor gram for detecting trace sulfadimidine of the present invention
To there is method the most loaded down with trivial details when detecting trace sulfadimidine to have taken prior art, and step is complicated etc. many lacks
Point, preferably improves sensitivity and the selectivity of detection, and the detection for trace sulfadimidine is prone to certainly
Dynamicization.
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:Fe3O4@rGO/ magnetic core electrode；C:MIP modified electrode；D: the MIP after eluted template
Modified electrode.
Fig. 2 a is the scanning electron microscope diagram of MIP modified electrode, and Fig. 2 b is that the MIP after wash-out modifies electricity
The scanning electron microscope diagram of pole.
Fig. 3 is standard absorption curve of the present invention.
Detailed description of the invention
Embodiment 1: the magnetic molecularly imprinted electrochemistry for detecting trace sulfadimidine of the present invention
The structure of sensor, it is characterised in that described magnetic molecularly imprinted electrochemical sensor is to make by the following method
Standby:
(1) process of magnetic core electrode:
After magnetic core glass-carbon electrode is put in the sulfuric acid of 0.2M activation 20min, successively by 1.0,0.3 and 0.05 μm
Alpha-alumina powder carry out surface finish process, with ultrapure water clean after dry, then electrode is placed in
The K of 5mM3[Fe(CN)6] in solution, in-0.2V～0.6V potential range, the speed with 100mV/s is carried out
Cyclic voltammetric (CV) scanning is until obtaining stable cyclic voltammogram.
(2) modification of magnetic core electrode:
Weigh 10mg magnetizing reduction Graphene Fe3O4@rGO is placed in ultrasonic disperse 10min, shape in 4mL water
Become 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 that to be configured to the sulfadimidine of 5mM in N, N-dimethyl pyrimidine molten
Liquid, Dopamine hydrochloride is dissolved in water and is configured to 10mM Dopamine hydrochloride solution；Pipette above-mentioned solution respectively each
0.1mL, utilizes PBS to regulate pH value, and after ultrasonically treated 20min, solution becomes faint yellow
Stand-by；
(4) structure of sensor:
Magnetic core electrode after modifying immerses in polymer fluid, uses cyclic voltammetry with 100 under-0.2V～0.6V
Scanning a fixing turn under the speed of mV/S, the eluent being placed in 0.2M hydrochloric acid-ethanol (1:2, V/V) is clear
Wash, obtain the magnetic molecularly imprinted electrochemical sensor of sulfadimidine.
Embodiment 2: the magnetic molecularly imprinted electrochemistry for detecting trace sulfadimidine of the present invention
The cyclic voltammetric of sensor characterizes
Owing to the trace hole in film can use K as the passage of electron transmission3[Fe(CN)6] it is probe, root
Size according to its electric current characterizes the surface nature of various electrodes.As it is shown in figure 1, Different electrodes is 5mM's
K3[Fe(CN)6] cyclic voltammogram significant difference in solution.Curve a is the cyclic voltammogram of naked magnetic core electrode,
Redox peak is obvious.Shown in curve b, when modifying one layer of Fe on magnetic glassy carbon electrode surface3O4@rGO is multiple
After compound, peak current has increase clearly, and this is due to Fe3O4@rGO composite conductivity is fine, energy
Promote the electron transmission of electrode surface, increase current signal.Electrode surface electricity shown in curve c, after modifying
After polymerization blotting membrane, it appeared that redox peak current is decreased obviously, because after electropolymerization MIPs, sensing
The electron transfer process of device is hindered.As shown in curve d, template molecule sulfadimidine is eluted,
Having hole to allow electronics transmit, signal recovers.
Embodiment 3: the magnetic molecularly imprinted electrochemistry for detecting trace sulfadimidine of the present invention
The ESEM of the different modifying electrode of sensing characterizes
Use ESEM, the microstructure of different modifying electrode is characterized.As shown in Figure 2 a, exist
Molecular engram film rear electrode smooth surface on electrode face finish, illustrates that imprinting effect is good；After wash-out,
Owing to template molecule is eluted, therefore leave many holes, therefore surface on this molecular engram film surface
Become coarse (seeing Fig. 2 b).
Embodiment 4: the range of linearity is tested with detection limit
With optimal conditions, by trace electrode in K3Fe(CN)6Solution carries out differential pulse voltammetry scanning, surveys
Determine oxidation peak current and be designated as I0Then trace electrode is immersed in the olaquindox solution of variable concentrations adsorbs identical
Time, the oxidation peak current recorded after absorption is designated as I, tests with relative peak current △ I (△ I=I0-I) retouch
State curent change.As it is shown on figure 3, in the concentration range that concentration is 10-200nM, △ I (μ A) and sulfanilamide (SN) two
First pyrimidine concentration C (nM) presents 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: reappearance and stability experiment
The reappearance of molecular imprinting electrochemical sensor is by measuring same a part of preparation under the same terms print
Apodized electrode is to carrying out DPV detection in the sulfadimidine solution of 100nM, relative standard deviation is 4.05%,
Show that trace electrode has good invertibity and reappearance.
The stability of sensor is also the key factor that whether good research sensor is, prepares 3 under the same conditions
The sensor of Zhi Xiangtong, is put in refrigerator preservation 2 weeks, the most respectively at the sulfadimidine to 100nM
Solution carries out DPV detection.End product finds that response current value is original 89% after showing two weeks, table
Bright sensor has preferable stability.
Embodiment 6: actual sample measures
Taking milk 2mL to be measured, under 3000rpm, centrifugal 10min, abandons butterfat, and ultra-pure water dilutes, and puts into trace
After electrode 10min, marking electrode is transferred in potassium ferricyanide test fluid, measures iron with differential pulse voltammetry
Potassium cyanide probe molecule current-responsive on trace electrode.Then standard addition method is used to be added thereto to necessarily
Detecting after the sulfadimidine of amount, measurement result is shown in Table 1.The rate of recovery of method is as shown in Table 1
95.9%-103.2%, relative standard deviation is 1.67%-3.28%.
Table 1 milk sample analysis
| Sequence number | Add scalar nM | Actually detected nM | The rate of recovery (%) | 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. for detecting a magnetic molecularly imprinted electrochemical sensor for trace sulfadimidine, its feature
Being, described magnetic molecularly imprinted electrochemical sensor is prepared by the following method:
(1) process of magnetic core electrode:
After magnetic core glass-carbon electrode is put in the sulfuric acid of 0.2M activation 20min, successively by 1.0,0.3 and 0.05 μm
Alpha-alumina powder carry out surface finish process, with ultrapure water clean after dry, then electrode is placed in
The K of 5mM3[Fe(CN)6] in solution, in-0.2V～0.6V potential range, the speed with 100mV/s is carried out
Cyclic voltammetric (CV) scanning is until obtaining stable cyclic voltammogram；
(2) modification of magnetic core electrode:
Weigh 10mg magnetizing reduction Graphene Fe3O4@rGO, is placed in ultrasonic disperse 10min in 4mL water,
Form dispersion liquid；Pipette the 5 μ careful drop coatings of L dispersion liquid in electrode surface with micropipette rifle, be placed in infrared lamp
Lower drying for standby；
(3) preparation of molecular engram polymer fluid:
Sulfadimidine is dissolved in that to be configured to the sulfadimidine of 5mM in N, N-dimethyl pyrimidine molten
Liquid, is dissolved in Dopamine hydrochloride water and is configured to 10mM Dopamine hydrochloride solution；Pipette above-mentioned solution respectively
Each 0.1mL, utilizes PBS to regulate pH value, and after ultrasonically treated 20min, solution becomes yellowish
Look stand-by；
(4) structure of sensor:
Magnetic core electrode after modifying immerses in polymer fluid, uses cyclic voltammetry with 100 under-0.2V～0.6V
Scan a fixing turn under the speed of mV/S, be placed in 0.2M hydrochloric acid-ethanol (1:2, V/V) eluent and clean,
Obtain the magnetic molecularly imprinted electrochemical sensor of sulfadimidine.
Magnetic molecularly imprinted electrochemical sensor the most according to claim 1, it is characterised in that: described step
Suddenly, in (3), PBS regulation pH value is 7.5.
Magnetic molecularly imprinted electrochemical sensor the most according to claim 1, it is characterised in that: described step
Suddenly, in (4), the scanning number of turns is 20 circles.
Magnetic molecularly imprinted electrochemical sensor the most according to claim 1, it is characterised in that: described step
Suddenly, in (4), eluent scavenging period is 20min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109254061A (en) * | 2018-11-05 | 2019-01-22 | 济南大学 | A kind of preparation method and application of Sulfa drugs molecule Electrochemiluminescsensor sensor |
| CN109342516A (en) * | 2018-11-05 | 2019-02-15 | 济南大学 | A kind of preparation method and application of Sulfa drugs molecule electrochemical sensor |
| 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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| WO2013061041A1 (en) * | 2011-10-24 | 2013-05-02 | The Secretary Of State For Business Innovation & Skills Of Her Majesty's Britannic Goverment | Electrochemical assay |
| 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 |
| CN105699470A (en) * | 2016-03-31 | 2016-06-22 | 肇庆学院 | Magnetic molecular imprinting electrochemical sensor for detecting trace sulfadimidine |
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2016
- 2016-04-01 CN CN201610206836.6A patent/CN105891290A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2013061041A1 (en) * | 2011-10-24 | 2013-05-02 | The Secretary Of State For Business Innovation & Skills Of Her Majesty's Britannic Goverment | Electrochemical assay |
| 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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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109254061A (en) * | 2018-11-05 | 2019-01-22 | 济南大学 | A kind of preparation method and application of Sulfa drugs molecule Electrochemiluminescsensor sensor |
| CN109342516A (en) * | 2018-11-05 | 2019-02-15 | 济南大学 | A kind of preparation method and application of Sulfa drugs molecule electrochemical sensor |
| 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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