CN105158236A - Preparation method of electrochemiluminescence sensor for detecting benzoapyrene - Google Patents
Preparation method of electrochemiluminescence sensor for detecting benzoapyrene Download PDFInfo
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- CN105158236A CN105158236A CN201510465264.9A CN201510465264A CN105158236A CN 105158236 A CN105158236 A CN 105158236A CN 201510465264 A CN201510465264 A CN 201510465264A CN 105158236 A CN105158236 A CN 105158236A
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Abstract
The invention relates to a preparation method of electrochemiluminescence sensor for detecting benzoapyrene, especially provides a preparation method of electrochemiluminescence sensor for detecting benzoapyrene based on grapheme/Ag/TiO2 nanotube (GR/Ag/TiO2 NTs) composite material. According to a dispensing method, GR/Ag/TiO2 NTs are modified on the electrode surface, TiO2 NTs is used as a luminescent material with more surface area and active sites, grapheme and silver nanoparticles can be used for catalyzing S2O8<2->, so that more electronic cavities are produced for improving the electron transfer rate of electrons on sensing interfaces and increasing electrochemiluminescence intensity, and the electrochemiluminescence sensor constructed based on the material has a higher sensitivity and a lower detection limit for detecting benzoapyrene.
Description
Technical field
The invention belongs to Electrochemiluminescsensor sensor technical field, be specifically related to a kind of preparation method detecting the Electrochemiluminescsensor sensor of benzo [a] pyrene.
Background technology
Palycyclic aromatic enjoys people to pay close attention to because having strong teratogenesis, carcinogenicity and mutagenicity.Benzo [a] pyrene is maximum at palycyclic aromatic family Poisoning, and has certain correlativity with the content of other palycyclic aromatic, therefore generally using the representative of benzo [a] pyrene as the potential carcinogenicity of monitoring palycyclic aromatic.Mainly liquid phase chromatography is comprised to the separation and detection technology of palycyclic aromatic, high resolution gas chromatography-fluorescence coupling technique, Gas chromatographyMass spectrometry at present.These methods need to carry out pre-service to sample to be analyzed usually, consuming time and cost is high, are difficult to realize real-time online and detect.Immunoassay is also limited to because lacking corresponding antibody.Electrogenerated chemiluminescence is highly sensitive because of it in recent decades, favorable reproducibility, and detection speed is fast, and device simply obtains the extensive concern of people.TiO
2be a kind of material with high light chemical stability, there is the advantages such as surface area is large, selecting property is good, high adsorption capacity.With TiO
2compare TiO
2nTs has larger specific surface area, can provide more avtive spot, becomes the focus of research in electrochemiluminescence and photochemiluminescence.Because palycyclic aromatic concentration is in the environment extremely low, sensor is therefore needed to have higher sensitivity, and simple TiO
2modified electrode is difficult to reach the requirement analyzed and measure.
The present invention adopts the TiO with more high surface area and avtive spot
2nTs and Graphene (GR) and Ag adulterate.GR has large surface area, the electro catalytic activity of good thermal conductivity, electric conductivity, structural stability and excellence, is that a kind of good host material is widely used in sensor.And Nano silver grain as a kind of metal nano material because the quantum effect, surface effect etc. of its uniqueness shows excellent PhotoelectrocatalytiPerformance Performance.The present invention obtains a kind of compound substance in conjunction with the character of GR and Nano silver grain.Not only can catalysis S under the synergy of GR and Nano silver grain
2o
8 2-produce more electron hole electronics can also be promoted at the electron transport rate of sensing interface thus increase ECL intensity.At S
2o
8 2-tiO is adsorbed in system
2benzo [a] pyrene on NTs surface is generated anthraquinone, along with excited state TiO by electron hole oxidation
2consumption cause its electrogenerated chemiluminescence intensity to reduce, realize the detection of benzo in aqueous systems [a] pyrene accordingly.This modified electrode manufacturing process is easy, good stability, has high sensitivity to benzo [a] pyrene.
Summary of the invention
The object of the present invention is to provide a kind of preparation method detecting the Electrochemiluminescsensor sensor of benzo [a] pyrene, especially based on GR/Ag/TiO
2the preparation method of the Electrochemiluminescsensor sensor of detection benzo [a] pyrene of NTs compound substance.
Technical scheme of the present invention is:
The preparation method of Electrochemiluminescsensor sensor of the present invention comprises the steps:
(1) TiO
2nanotube (TiO
2nTs) preparation;
(2) Ag/TiO
2the preparation of NTs;
(3) Graphene/Ag/TiO
2nTs (GR/Ag/TiO
2nTs) preparation of solution;
(4) drop-coating is utilized to prepare Electrochemiluminescsensor sensor and for detecting benzo [a] pyrene.
Described step (1) TiO
2nanotube (TiO
2nTs) preparation, specifically comprises the following steps:
A takes 0.6gP25-TiO
2join ultrasonic 30min in 60mL10mol/LNaOH solution, then lucifuge stirs 12h and moves in polytetrafluoroethyllining lining autoclave after fully mixing, and under 150 ° of C, constant temperature keeps 48h, naturally cools to room temperature, centrifugally obtains solid sample;
Above-mentioned sample is first washed till neutrality with ultrapure water by b, repeatedly clean to the pH of pH close to HCl solution with 0.01mLHCl solution again, finally repeatedly clean with ultrapure water, until the pH value of the aqueous solution washed out is close to centrifugal again after neutrality, by after the dry 12h of the solid sample obtained 80 ° of C in drying box again in muffle furnace 350 ° of C calcining at constant temperature 30min obtain TiO
2nTs, grinds for subsequent use after naturally cooling to room temperature.
Described step (2) Ag/TiO
2the preparation of NTs, specifically comprises the following steps:
Get 2.0mL0.05mol/LAgNO
3join in 30mL ethylene glycol with 1.0mL0.4mol/LKOH solution, then add the obtained TiO of 0.1g step (1)
2nTs ultrasound wave process 20min.Subsequently mixed solution to be transferred in polytetrafluoroethyllining lining autoclave constant temperature under 120 ° of C and to keep 12h, after naturally cooling to room temperature, 9000 leave heart 15min, wash 5 times with acetone, under 50 ° of C, obtain solid Ag/TiO after vacuum drying 6h
2nTs.
Described step (3) Graphene/Ag/TiO
2nTs (GR/Ag/TiO
2nTs) preparation of solution, specifically comprises the following steps:
The preparation of a reduced graphene: the graphene oxide water solution of getting 20mL0.5mg/mL, adds dense NH successively
3(300 μ L) and hydrazine hydrate (20 μ L), stirring in water bath 3.5h at 60 DEG C, the mixed solution 9000 obtained leaves heart 10min, with milli-Q water 3 times, under 50 ° of C, obtains GR after vacuum drying 6h;
The GR that b takes 2mg step (3) a obtained is dissolved into ultrasonic disperse in 2mL ultrapure water, adds the Ag/TiO that 2mg step (2) is obtained afterwards
2nTs continuation is ultrasonic processes to obtain finely dispersed GR/Ag/TiO
2nTs solution.
Described step (4) utilizes drop-coating to prepare Electrochemiluminescsensor sensor and for detecting benzo [a] pyrene, specifically comprises the following steps:
A uses the Al of 1.0 μm, 0.3 μm, 0.05 μm successively
2o
3burnishing powder polishing diameter is the glass-carbon electrode (GCE) of 4mm, ultrasonic cleaning 3min in ethanol and ultrapure water respectively, and nitrogen dries up;
B gets the obtained GR/Ag/TiO of 10 μ L steps (3)
2nTs solution is added drop-wise to the GCE that handles well on the surface, naturally dries rear ultrapure water 3 times, namely obtains GR/Ag/TiO
2nTs/GCE Electrochemiluminescsensor sensor;
C is with GR/Ag/TiO
2nTs/GCE is working electrode, and Ag/AgCl electrode is contrast electrode, and platinum electrode is to electrode.In the electrolytic cell of 10mLPBS (pH6.0) solution containing 0.1mol/L potassium persulfate, utilize electroluminescent technology to detect benzo [a] pyrene to the impact of working electrode electrogenerated chemiluminescence intensity, linear according to the logarithm of relative electrogenerated chemiluminescence intensity and benzo [a] pyrene concentration, drawing curve.
Useful achievement of the present invention
(1) the present invention utilizes GR/Ag/TiO
2nTs/GCE compound substance modified electrode, TiO
2nTs has larger surface area and can provide more avtive spot, makes TiO in this invention under the synergy of GR and Nano silver grain simultaneously
2nTs is containing coreagent S
2o
8 2-system in there is stronger electrogenerated chemiluminescence intensity, significantly increase the sensitivity of electrode;
(2) the present invention utilizes drop-coating to prepare GR/Ag/TiO
2nTs/GCE compound substance modified glassy carbon electrode, electrode fabrication is comparatively simple, and material price is cheap, good stability;
(3) Electrochemiluminescsensor sensor prepared of the present invention is for the detection of benzo [a] pyrene, and simple to operate, the range of linearity is wide, and detection limit is low, can realize simple, quick, the highly sensitive detection to benzo [a] pyrene.The range of linearity is 5.0 × 10
-12mol/L ~ 1.0 × 10
-9mol/L, detects and is limited to 2.3 × 10
-13mol/L.
accompanying drawing illustrates:
Figure 1 shows that TiO of the present invention
2the transmission electron microscope figure (TEM) of NTs;
Figure 2 shows that the present invention adds the electrogenerated chemiluminescence figure of modified electrode after different concentrations of benzo [a] pyrene;
Figure 3 shows that the relative electrogenerated chemiluminescence intensity of the present invention and lg
clinear relationship chart.
Wherein, benzo [a] pyrene concentration 0,5.0 × 10 is represented respectively by a to f in Fig. 2
-12, 5.0 × 10
-11, 1.0 × 10
-10, 5.0 × 10
-10, 1.0 × 10
-9.
embodiment:
In order to understand the present invention better, describe technical scheme of the present invention in detail with instantiation below, but the present invention is not limited thereto.
Embodiment 1 one kinds detects the preparation method of the Electrochemiluminescsensor sensor of benzo [a] pyrene
Step 1. prepares TiO
2nanotube (TiO
2nTs): take 0.6gP25-TiO
2join ultrasonic 30min in 60mL10mol/LNaOH solution, then lucifuge stirs 12h and moves in polytetrafluoroethyllining lining autoclave after fully mixing, and under 150 ° of C, constant temperature keeps 48h, naturally cools to room temperature, centrifugally obtains solid sample; Above-mentioned sample is first washed till neutrality with ultrapure water, repeatedly clean to the pH of pH close to HCl solution with 0.01mLHCl solution again, finally repeatedly clean with ultrapure water, until the pH value of the aqueous solution washed out is close to centrifugal again after neutrality, by after the dry 12h of the solid sample obtained 80 ° of C in drying box again in muffle furnace 350 ° of C calcining at constant temperature 30min obtain TiO
2nTs, grinds for subsequent use after naturally cooling to room temperature, obtained sample is carried out tem analysis, and result, see accompanying drawing 1, is wound around and unordered tubular structure as we can see from the figure mutually.
Step 2. prepares Ag/TiO
2nTs: get 2.0mL0.05mol/LAgNO
3join in 30mL ethylene glycol with 1.0mL0.4mol/LKOH solution, then add the obtained TiO of 0.1g step (1)
2nTs ultrasound wave process 20min; Subsequently mixed solution to be transferred in polytetrafluoroethyllining lining autoclave constant temperature under 120 ° of C and to keep 12h, after naturally cooling to room temperature, 9000 leave heart 15min, wash 5 times with acetone, under 50 ° of C, obtain solid Ag/TiO after vacuum drying 6h
2nTs.
Step 3. prepares Graphene/Ag/TiO
2nTs (GR/Ag/TiO
2nTs) solution:
The preparation of a reduced graphene: the graphene oxide water solution of getting 20mL0.5mg/mL, adds dense NH successively
3(300 μ L) and hydrazine hydrate (20 μ L), stirring in water bath 3.5h at 60 DEG C, the mixed solution 9000 obtained leaves heart 10min, with milli-Q water 3 times, under 50 ° of C, obtains GR after vacuum drying 6h;
The GR that b takes 2mg step (3) a obtained is dissolved into ultrasonic disperse in 2mL ultrapure water, adds the Ag/TiO that 2mg step (2) is obtained afterwards
2nTs continuation is ultrasonic processes to obtain finely dispersed GR/Ag/TiO
2nTs solution.
Step 4. utilizes drop-coating to prepare Electrochemiluminescsensor sensor and for detecting benzo [a] pyrene: the Al using 1.0 μm, 0.3 μm, 0.05 μm successively
2o
3burnishing powder polishing diameter is the glass-carbon electrode (GCE) of 4mm, ultrasonic cleaning 3min in ethanol and ultrapure water respectively, and nitrogen dries up; Get the GR/Ag/TiO that 10 μ L steps (3) are obtained
2nTs solution is added drop-wise to the GCE that handles well on the surface, naturally dries rear ultrapure water 3 times, namely obtains GR/Ag/TiO
2nTs/GCE Electrochemiluminescsensor sensor.
Step 5. is that carry out of working electrode to benzo [a] pyrene standard model detects with the sensor that step 4 obtains:
A in the electrolytic cell of 10mLPBS (pH6.0) solution containing 0.1mol/L potassium persulfate, with GR/Ag/TiO
2nTs/GCE is working electrode, and Ag/AgCl electrode is contrast electrode, and platinum electrode is to electrode; Experiment is carried out on MPI-B type multiparameter chemiluminescence analysis test macro, and its attached computer software is made for the acquisition and processing of experimental data; At photomultiplier transit voltage 600V, sweep interval-2.0 ~ 0.4V, sweep velocity 100mV/s carry out electrogenerated chemiluminescence biography (ECL) and detect, and record ECL signal, measures ECL intensity, be blank ECL intensity
i 0;
B microsyringe is got a certain amount of benzo [a] pyrene solution and is joined in electrolytic cell, carries out ECL detection, and record ECL signal, measures ECL intensity
i 1, calculate the difference DELTA adding ECL after benzo [a] pyrene
i 1(
i 1-
i 0); According to said method, add benzo [a] the pyrene standard solution of variable concentrations, ECL figure is shown in Fig. 1.According to the electrogenerated chemiluminescence intensity of gained and the relation of benzo [a] pyrene concentration, drawing curve, obtains relative electrogenerated chemiluminescence intensity Δ
i/
i 0with the logarithm (lg of benzo [a] pyrene concentration
c) linear relationship see Fig. 2, as shown in Figure 2, benzo [a] pyrene is 5.0 × 10
-12~ 1.0 × 10
-9in the concentration range of mol/L, Δ
i/
i 0with lg
cpresent good linear correlation, linear equation is Δ
i/
i 0=-2.719-0.233lg
c, linearly dependent coefficient is 0.9958, detects and is limited to 2.3 × 10
-13mol/L.
The detection of benzo [a] the pyrene sample of step 6. unknown concentration: in the electrolytic cell of 10mLPBS (pH6.0) solution containing 0.1mol/L potassium persulfate, with GR/Ag/TiO
2nTs/GCE is working electrode, and Ag/AgCl electrode is contrast electrode, and platinum electrode is to electrode; Experiment is carried out on MPI-B type multiparameter chemiluminescence analysis test macro, and its attached computer software is made for the acquisition and processing of experimental data; At photomultiplier transit voltage 600V, sweep interval-2.0 ~ 0.4V, sweep velocity 100mV/s carry out ECL detection, record ECL signal; Then add a certain amount of solution to be measured, scan under the same terms, record ECL signal, obtains relative ECL intensities Δ
i/
i 0, by Δ
i/
i 0bring step 5 gained linear equation into, the concentration calculating benzo [a] pyrene in liquid to be measured can be asked.
Claims (5)
1. detect a preparation method for the Electrochemiluminescsensor sensor of benzo [a] pyrene, it is characterized in that, comprise the following steps:
(1) TiO
2nanotube (TiO
2nTs) preparation;
(2) Ag/TiO
2the preparation of NTs;
(3) Graphene/Ag/TiO
2nTs (GR/Ag/TiO
2nTs) preparation of solution;
(4) drop-coating is utilized to prepare Electrochemiluminescsensor sensor and for detecting benzo [a] pyrene.
2. one according to claim 1 detects the preparation method of the Electrochemiluminescsensor sensor of benzo [a] pyrene, it is characterized in that described step (1) is specially:
A takes 0.6gP25-TiO
2join ultrasonic 30min in 60mL10mol/LNaOH solution, then lucifuge stirs 12h and moves in polytetrafluoroethyllining lining autoclave after fully mixing, and under 150 ° of C, constant temperature keeps 48h, naturally cools to room temperature, centrifugally obtains solid sample;
Above-mentioned sample is first washed till neutrality with ultrapure water by b, repeatedly clean to the pH of pH close to HCl solution with 0.01mLHCl solution again, finally repeatedly clean with ultrapure water, until the pH value of the aqueous solution washed out is close to centrifugal again after neutrality, by after the dry 12h of the solid sample obtained 80 ° of C in drying box again in muffle furnace 350 ° of C calcining at constant temperature 30min obtain TiO
2nTs, grinds for subsequent use after naturally cooling to room temperature.
3. one according to claim 1 detects the preparation method of the Electrochemiluminescsensor sensor of benzo [a] pyrene, it is characterized in that described step (2) is specially:
Get 2.0mL0.05mol/LAgNO
3join in 30mL ethylene glycol with 1.0mL0.4mol/LKOH solution, then add the obtained TiO of 0.1g step (1)
2nTs ultrasound wave process 20min; Subsequently mixed solution to be transferred in polytetrafluoroethyllining lining autoclave constant temperature under 120 ° of C and to keep 12h, after naturally cooling to room temperature, 9000 leave heart 15min, wash 5 times with acetone, under 50 ° of C, obtain solid Ag/TiO after vacuum drying 6h
2nTs.
4. one according to claim 1 detects the preparation method of the Electrochemiluminescsensor sensor of benzo [a] pyrene, it is characterized in that described step (3) is specially:
The preparation of a reduced graphene: the graphene oxide water solution of getting 20mL0.5mg/mL, adds dense NH successively
3(300 μ L) and hydrazine hydrate (20 μ L), stirring in water bath 3.5h at 60 DEG C, the mixed solution 9000 obtained leaves heart 10min, with milli-Q water 3 times, under 50 ° of C, obtains GR after vacuum drying 6h;
The GR that b takes 2mg step (3) a obtained is dissolved into ultrasonic disperse in 2mL ultrapure water, adds the Ag/TiO that 2mg step (2) is obtained afterwards
2nTs continuation is ultrasonic processes to obtain finely dispersed GR/Ag/TiO
2nTs solution.
5. one according to claim 1 detects the preparation method of the Electrochemiluminescsensor sensor of benzo [a] pyrene, it is characterized in that described step (4) is specially:
A uses the Al of 1.0 μm, 0.3 μm, 0.05 μm successively
2o
3burnishing powder polishing diameter is the glass-carbon electrode (GCE) of 4mm, ultrasonic cleaning 3min in ethanol and ultrapure water respectively, and nitrogen dries up;
B gets the obtained GR/Ag/TiO of 10 μ L steps (3)
2nTs solution is added drop-wise to the GCE that handles well on the surface, naturally dries rear ultrapure water 3 times, namely obtains GR/Ag/TiO
2nTs/GCE Electrochemiluminescsensor sensor;
C is with GR/Ag/TiO
2nTs/GCE is working electrode, Ag/AgCl electrode is contrast electrode, platinum electrode is to electrode, 10mLPBS(pH6.0 containing 0.1mol/L potassium persulfate) solution electrolytic cell in utilize electroluminescent technology detect benzo [a] pyrene on the impact of working electrode electrogenerated chemiluminescence intensity, linear according to the logarithm of relative electrogenerated chemiluminescence intensity and benzo [a] pyrene concentration, drawing curve.
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