CN103454333A - Electrochemical detection method for pesticide imidacloprid based on polypyrrole/reduced graphene oxide (PPy/RGO) modified glassy carbon electrode - Google Patents
Electrochemical detection method for pesticide imidacloprid based on polypyrrole/reduced graphene oxide (PPy/RGO) modified glassy carbon electrode Download PDFInfo
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Abstract
The invention discloses an electrochemical detection method for a pesticide imidacloprid based on a polypyrrole/reduced graphene oxide (PPy/RGO) modified glassy carbon electrode. The method comprises the following steps: firstly, carrying out electrochemical reduction to prepare the polypyrrole/reduced graphene oxide (PPy/RGO) modified glassy carbon electrode; and secondly, utilizing the prepared PPy/RGO modified glassy carbon electrode to the electrochemical detection of the pesticide imidacloprid. The PPy/RGO modified glassy carbon electrode provided by the invention has high sensitivity, good stability, wide linear range and low detection limit on the detection of the imidacloprid.
Description
Technical field
The invention belongs to electrochemical analysis detection technique field, relate to a kind of based on the PPy/RGO modified electrode electrochemical detection method to pesticide imidacloprid.
Background technology
Polypyrrole is a kind of important conducting polymer be widely studied, have manufacture simple, high conductivity, good biocompatibility, the characteristics such as cost is low.Take the pyrroles as monomer, usually can make conductive membrane by electrochemically oxidative polymerization, also can synthesize by the electrochemical anodic oxidation pyrroles.Under the existence of the amine groups on pyrrole ring (NH-), may cause the enhancing of biomolecule detection.Simultaneously, polypyrrole also can be used for electrode material, electrocatalysis material, conducting polymer composite material of modified electrode, the accumulator of ion detection, photoelectrochemical cell etc.
Graphene is a kind of monoatomic carbon atom, recent years, it is found that the two dimensional crystal of carbon atom has very high chemical stability, good electric conductivity and large other features such as specific surface area.Graphene oxide (GO) is most important Graphene derivant, contains a large amount of oxygen-containing functional groups and makes it to be dispersed in water at an easy rate.Can adopt chemical reduction method, thermal reduction and electrochemical reducing preparation by graphene oxide containing the oxygen graphene oxide.Redox graphene has some characteristics of Graphene, also has special performances such as preparing simply, be convenient to modification, and some materials in environment are had to high sensitive response.
Imidacloprid chemistry 1-[(6-chloro-3-pyridyl base by name) methyl]-N-nitroimidazole alkane-2-base amine, be a kind of efficient, low toxicity, interior absorption is strong, the longevity of residure is long, residual quantity is low broad spectrum insecticide, there is stomach toxicity and action of contace poison.Widespread use due to Imidacloprid in agricultural production, make and become more and more important detecting residual Imidacloprid aspect food security and environmental protection.The detection method of Imidacloprid has high performance liquid chromatography, liquid chromatography-mass spectrography and gas chromatography-mass spectrography etc., however the shortcomings such as preprocessor that these instrument analytical methods have is consuming time, cost is high, complicated.Electrochemical method is because it is simple to operate, highly sensitive, and analysis cost is low to be polluted and more and more paid close attention to low environment.For the sensitivity and the selectivity that improve Electrochemical Detection, the glass-carbon electrode of many modifications has been in the news for detecting Imidacloprid.The people such as Wu Qiuju (Electrochemical determination of imidacloprid using poly (carbazole)/chemically reduced graphene oxide modified glassy carbon electrode, Sensors and Actuators B:Chemical, 183 (2013) 102-109) studied the electrochemical behavior of Imidacloprid on the graphene oxide modified glassy carbon electrode of polycarbazole/electronation.And the preparation of the graphene oxide modified glassy carbon electrode of polycarbazole/electronation is complicated, in polymerization process, can use harmful boron trifluoride ether solution.Therefore, develop a kind of new and effective, preparation is simple, environmental friendliness and harmless modified electrode are used for detecting Imidacloprid has become new development trend.
Summary of the invention
The object of the present invention is to provide the application of the wide electrochemical sensor polypyrrole of a kind of highly sensitive, good stability, the range of linearity/redox graphene modified glassy carbon electrode to the Imidacloprid Electrochemical Detection.
The technical solution that realizes the object of the invention is:
A kind of based on the PPy/RGO modified glassy carbon electrode electrochemical detection method to pesticide imidacloprid, said method comprising the steps of:
(1) preparation of PPy/RGO modified glassy carbon electrode: pure pyrrole monomer is added drop-wise in the dispersion liquid of graphene oxide, then ultrasonic half an hour, obtain the mixed solution that contains pyrrole monomer and graphene oxide, the glass-carbon electrode of clean preparation is placed in to mixed solution, potential region is-0.2 ~ 1.0 V cyclic voltammetric polymerization 5 ~ 30 circles, sweeping speed is 100 mV/s, obtains the glass-carbon electrode that polypyrrole/graphene oxide is modified; The glass-carbon electrode that the polypyrrole that obtains/graphene oxide is modified is placed in the phosphate buffered solution of pH=7, and potential region is 0 ~-1.7 V cyclic voltammetry scan 5 ~ 10 circles, and sweeping speed is 100 mV/s, obtains the PPy/RGO modified glassy carbon electrode;
(2) PPy/RGO modified electrode step (1) obtained is positioned in the buffer solution of pH value 2.8 ~ 7.5, logical nitrogen 5-20 minute, add a certain amount of Imidacloprid, use cyclic voltammetry, sweep velocity is that 10 ~ 200 mV/s and differential pulse voltammetry detect the electrochemical response of PPy/RGO modified electrode to pesticide imidacloprid.
Wherein, in step (1), pure pyrrole monomer consumption is 10-20 μ L; The graphene oxide consumption is 10 ml, and concentration is 0.5-5mg/mL.
The described buffer solution of step (2) is citric acid/sodium hydrogen phosphate system.
The amount of the described Imidacloprid of step (2) is 1-100 μ mol/L.
Compared with prior art, its remarkable advantage is in the present invention: electroactive better, the electric active area of the graphene oxide modified glassy carbon electrode of (1) polypyrrole/electrochemical reduction is larger, electron transfer rate is faster.Why having above advantage, be because polypyrrole has good electric conductivity, and then the graphene oxide of the electrochemical reduction of polypyrrole functional has larger surface area and roughness.(2) the graphene oxide modified glassy carbon electrode of polypyrrole/electrochemical reduction is for the detection of pesticide imidacloprid, and the graphene oxide modified electrode of polypyrrole/electrochemical reduction has high sensitivity, good stability, the wide range of linearity and low detection limit.
Below in conjunction with accompanying drawing, the present invention is described in further detail.
The accompanying drawing explanation
The scanning electron microscope (SEM) photograph of PPy/RGO modified glassy carbon electrode in Fig. 1 embodiment of the present invention 1.
The AC impedance spectrogram of Different electrodes in Fig. 2 embodiment of the present invention 1.
The cyclic voltammetric response (A) that in Fig. 3 embodiment of the present invention 1, Different electrodes detects Imidacloprid and differential pulse voltammetry response (B).
PPy/RGO modified glassy carbon electrode cyclic voltammetry curve (A) of (be respectively from a to k 10,15,20,25,30,40,50,60,70,80,90,100,150,200mV/s) under difference is swept speed in Fig. 4 embodiment of the present invention 1, figure B and C are the linear relationship of sweeping speed and reduction peak current.
The cyclic voltammetry curve that in Fig. 5 embodiment of the present invention 1, the PPy/RGO modified glassy carbon electrode (is respectively 2.7,3.2,4.1,5,5.9,6.7,7.2) under different pH values from a to g, the relation that interior illustration is pH and reduction peak current.
In Fig. 6 embodiment of the present invention 1, PPy/RGO alkene modified glassy carbon electrode detects the differential pulse voltammetry curve (A) of variable concentrations Imidacloprid, the linear relationship that figure B is Imidacloprid concentration and reduction peak current.
Embodiment
The following examples can make the present invention of those skilled in the art comprehend.
Embodiment 1
The electrochemical detection method of PPy/RGO modified glassy carbon electrode to Imidacloprid, is characterized in that, comprises the following steps:
(1) preparation of polypyrrole/redox graphene modified glassy carbon electrode (PPy/RGO): the pure pyrrole monomer of 10 μ L is added drop-wise in the dispersion liquid that 10 ml graphene oxide concentration are 1mg/mL, then ultrasonic half an hour, obtain the mixed solution that contains pyrrole monomer and graphene oxide.The glass-carbon electrode of clean preparation is placed in to mixed solution, and potential region is-0.2 ~ 1.0 V cyclic voltammetric polymerization 10 circles, and sweeping speed is 100 mV/s, obtains the glass-carbon electrode that polypyrrole/graphene oxide is modified.The glass-carbon electrode that the polypyrrole that obtains/graphene oxide is modified is placed in the phosphate buffered solution of pH=7, and potential region is 0 ~-1.7 V cyclic voltammetry scan 10 circles, and sweeping speed is 100 mV/s, obtains the PPy/RGO modified glassy carbon electrode.
(2) PPy/RGO modified electrode step (1) obtained is positioned in the citric acid/disodium hydrogen phosphate buffer solution of pH value 6.7, logical nitrogen 20 minutes, the Imidacloprid that adds 100 μ mol/L, used cyclic voltammetry (sweep velocity is 100 mV/s) and differential pulse voltammetry to detect the electrochemical response of PPy/RGO modified electrode to pesticide imidacloprid.
As the scanning electron microscope (SEM) photograph that Fig. 1 is the PPy/RGO modified glassy carbon electrode, from scheming, can find out, the graphene oxide of polypyrrole/electrochemical reduction has large specific surface area and coarse surface, and is uniformly dispersed.
As shown in Figure 2, from half circular diameter of high frequency, glass-carbon electrode GCE is at [Fe (CN)
6]
3-/4-characterize the resistance maximum in liquid, polypyrrole/graphene oxide modified glassy carbon electrode takes second place, the resistance minimum of the graphene oxide modified glassy carbon electrode PPy/RGO of polypyrrole/electrochemical reduction.Show that the PPy/RGO modified electrode has better electric conductivity and electron transfer ability faster.
As shown in Figure 3, the graphene oxide modified glassy carbon electrode PPy/RGO of polypyrrole/electrochemical reduction detects and does not have the redox peak (the curve c in A, B figure) to occur at blank buffer solution, no matter and the curve b in GCE(A, B figure) or modified electrode (curve in A, B figure a) all only has an irreversible reduction peak in the buffer solution that contains 100 μ mol/L Imidacloprids.With GCE, compare, the reduction potential corrigendum of modified electrode, and also peak current strengthens significantly.To Imidacloprid, reduction has the sensitivity of more excellent electro catalytic activity and Geng Gao to this phenomenon explanation modified electrode, makes the PPy/RGO modified glassy carbon electrode can be used as a kind of electrochemical sensor, detects quickly and easily Imidacloprid.
As shown in Figure 4, along with sweeping fast increase, reduction peak current increases gradually, and the speed of sweeping of final Selective determination is 100 mV/s.Can find out from figure B, sweep fast square root and reduction peak current linear, show to sweep under speed low, the reduction reaction of Imidacloprid on the modified electrode surface is a diffusion controlled process.Can find out from figure C, sweep speed and reduction peak current linear, show under height is swept speed, the reduction reaction of Imidacloprid on the modified electrode surface is an absorption and control process.
As shown in Figure 5, the cyclic voltammetry curve of PPy/RGO modified electrode under different pH values, the relation that interior illustration is pH and reduction peak current.Along with the increase of pH value, reduction peak current first increases rear decline, and the pH value of final Selective determination is 6.7.
As shown in Figure 6, the Imidacloprid of variable concentrations adds respectively in sodium hydrogen phosphate/citrate buffer solution of pH 7.0, uses the PPy/RGO modified electrode to carry out differential pulse voltammetry mensuration to Imidacloprid.Result shows that this modified electrode has good linear relationship, significant sensitivity, the wide range of linearity and low detectability to Imidacloprid.
The electrochemical detection method of PPy/RGO modified glassy carbon electrode to Imidacloprid, is characterized in that, comprises the following steps:
(1) preparation of polypyrrole/redox graphene modified glassy carbon electrode (PPy/RGO): the pure pyrrole monomer of 15 μ L is added drop-wise in the dispersion liquid that 10 ml graphene oxide concentration are 5mg/mL, then ultrasonic half an hour, obtain the mixed solution that contains pyrrole monomer and graphene oxide.The glass-carbon electrode of clean preparation is placed in to mixed solution, and potential region is-0.2-1.0 V cyclic voltammetric polymerization 5 circles, and sweeping speed is 100 mV/s, obtains the glass-carbon electrode that polypyrrole/graphene oxide is modified.The glass-carbon electrode that the polypyrrole that obtains/graphene oxide is modified is placed in the phosphate buffered solution of pH=7, and potential region is 0 ~-1.7 V cyclic voltammetry scan 5 circles, and sweeping speed is 100 mV/s, obtains the PPy/RGO modified glassy carbon electrode.
(2) PPy/RGO modified electrode step (1) obtained is positioned in the citric acid/disodium hydrogen phosphate buffer solution of pH value 7.5, logical nitrogen 10 minutes, the Imidacloprid that adds 1 μ mol/L, used cyclic voltammetry (sweep velocity is 200 mV/s) and differential pulse voltammetry to detect the electrochemical response of PPy/RGO modified electrode to pesticide imidacloprid.
The electrochemical detection method of PPy/RGO modified glassy carbon electrode to Imidacloprid, is characterized in that, comprises the following steps:
(1) preparation of polypyrrole/redox graphene modified glassy carbon electrode (PPy/RGO): the pure pyrrole monomer of 20 μ L is added drop-wise in the dispersion liquid that 10 ml graphene oxide concentration are 0.5mg/mL, then ultrasonic half an hour, obtain the mixed solution that contains pyrrole monomer and graphene oxide.The glass-carbon electrode of clean preparation is placed in to mixed solution, and potential region is-0.2 ~ 1.0 V cyclic voltammetric polyase 13 0 circles, and sweeping speed is 100 mV/s, obtains the glass-carbon electrode that polypyrrole/graphene oxide is modified.The glass-carbon electrode that the polypyrrole that obtains/graphene oxide is modified is placed in the phosphate buffered solution of pH=7, and potential region is 0 ~-1.7 V cyclic voltammetry scan 10 circles, and sweeping speed is 100 mV/s, obtains the PPy/RGO modified glassy carbon electrode.
(2) PPy/RGO modified electrode step (1) obtained is positioned in the citric acid/disodium hydrogen phosphate buffer solution of pH value 2.8, logical nitrogen 5 minutes, the Imidacloprid that adds 50 μ mol/L, used cyclic voltammetry (sweep velocity is 10 mV/s) and differential pulse voltammetry to detect the electrochemical response of PPy/RGO modified electrode to pesticide imidacloprid.
Embodiment 4
The electrochemical detection method of PPy/RGO modified glassy carbon electrode to Imidacloprid, is characterized in that, comprises the following steps:
(1) preparation of polypyrrole/redox graphene modified glassy carbon electrode (PPy/RGO): the pure pyrrole monomer of 20 μ L is added drop-wise in the dispersion liquid that 10 ml graphene oxide concentration are 1mg/mL, then ultrasonic half an hour, obtain the mixed solution that contains pyrrole monomer and graphene oxide.The glass-carbon electrode of clean preparation is placed in to mixed solution, and potential region is-0.2 ~ 1.0 V cyclic voltammetric polymerization 20 circles, and sweeping speed is 100 mV/s, obtains the glass-carbon electrode that polypyrrole/graphene oxide is modified.The glass-carbon electrode that the polypyrrole that obtains/graphene oxide is modified is placed in the phosphate buffered solution of pH=7, and potential region is 0 ~-1.7 V cyclic voltammetry scan 8 circles, and sweeping speed is 100 mV/s, obtains the PPy/RGO modified glassy carbon electrode.
(2) PPy/RGO modified electrode step (1) obtained is positioned in the citric acid/disodium hydrogen phosphate buffer solution of pH value 7.5, logical nitrogen 10 minutes, the Imidacloprid that adds 1 μ mol/L, used cyclic voltammetry (sweep velocity is 100 mV/s) and differential pulse voltammetry to detect the electrochemical response of PPy/RGO modified electrode to pesticide imidacloprid.
Embodiment 5
The electrochemical detection method of PPy/RGO modified glassy carbon electrode to Imidacloprid, is characterized in that, comprises the following steps:
(1) preparation of polypyrrole/redox graphene modified glassy carbon electrode (PPy/RGO): the pure pyrrole monomer of 10 μ L is added drop-wise in the dispersion liquid that 10 ml graphene oxide concentration are 0.5mg/mL, then ultrasonic half an hour, obtain the mixed solution that contains pyrrole monomer and graphene oxide.The glass-carbon electrode of clean preparation is placed in to mixed solution, and potential region is-0.2 ~ 1.0 V cyclic voltammetric polymerization 10 circles, and sweeping speed is 100 mV/s, obtains the glass-carbon electrode that polypyrrole/graphene oxide is modified.The glass-carbon electrode that the polypyrrole that obtains/graphene oxide is modified is placed in the phosphate buffered solution of pH=7, and potential region is 0 ~-1.7 V cyclic voltammetry scan 5 circles, and sweeping speed is 100 mV/s, obtains the PPy/RGO modified glassy carbon electrode.
(2) PPy/RGO modified electrode step (1) obtained is positioned in the citric acid/disodium hydrogen phosphate buffer solution of pH value 6.7, logical nitrogen 20 minutes, the Imidacloprid that adds 100 μ mol/L, used cyclic voltammetry (sweep velocity is 100 mV/s) and differential pulse voltammetry to detect the electrochemical response of PPy/RGO modified electrode to pesticide imidacloprid.
Claims (4)
- One kind based on the PPy/RGO modified glassy carbon electrode electrochemical detection method to pesticide imidacloprid, it is characterized in that, said method comprising the steps of:(1) preparation of PPy/RGO modified glassy carbon electrode: pure pyrrole monomer is added drop-wise in the dispersion liquid of graphene oxide, then ultrasonic half an hour, obtain the mixed solution that contains pyrrole monomer and graphene oxide, the glass-carbon electrode of clean preparation is placed in to mixed solution, potential region is-0.2 ~ 1.0 V cyclic voltammetric polymerization 5 ~ 30 circles, sweeping speed is 100 mV/s, obtains the glass-carbon electrode that polypyrrole/graphene oxide is modified; The glass-carbon electrode that the polypyrrole that obtains/graphene oxide is modified is placed in the phosphate buffered solution of pH=7, and potential region is 0 ~-1.7 V cyclic voltammetry scan 5 ~ 10 circles, and sweeping speed is 100 mV/s, obtains the PPy/RGO modified glassy carbon electrode;(2) PPy/RGO modified electrode step (1) obtained is positioned in the buffer solution of pH value 2.8 ~ 7.5, logical nitrogen 5-20 minute, add a certain amount of Imidacloprid, use cyclic voltammetry, sweep velocity is that 10 ~ 200 mV/s and differential pulse voltammetry detect the electrochemical response of PPy/RGO modified electrode to pesticide imidacloprid.
- 2. electrochemical detection method according to claim 1, it is characterized in that: in step (1), pure pyrrole monomer consumption is 10-20 μ L; The graphene oxide consumption is 10 ml, and concentration is 0.5-5mg/mL.
- 3. electrochemical detection method according to claim 1, it is characterized in that: the described buffer solution of step (2) is citric acid/sodium hydrogen phosphate system.
- 4. electrochemical detection method according to claim 1, it is characterized in that: the amount of the described Imidacloprid of step (2) is 1-100 μ mol/L.
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