CN106323950A - Preparing method for sensor for detecting organophosphorus pesticide residues - Google Patents
Preparing method for sensor for detecting organophosphorus pesticide residues Download PDFInfo
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- CN106323950A CN106323950A CN201610650613.9A CN201610650613A CN106323950A CN 106323950 A CN106323950 A CN 106323950A CN 201610650613 A CN201610650613 A CN 201610650613A CN 106323950 A CN106323950 A CN 106323950A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/76—Chemiluminescence; Bioluminescence
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Abstract
The invention discloses a preparing method for an electrogenerated chemiluminescence sensor for detecting organophosphorus pesticide residues with a paper battery as power. The preparing process of the paper battery includes the steps that hydrophobic wax patterns are designed and printed as shown in the drawings; a filling area, a salt bridge area, an electrolyte area, a battery area and a connecting line area are established; the paper battery is assembled. The preparing process of the electrogenerated chemiluminescence sensor for detecting organophosphorus pesticide residues includes the steps of electrode pretreating, electrode modifying and detecting. The sensor is simple in preparing method, the paper battery serves as power, the cost is low, and the electrogenerated chemiluminescence sensor is of great significance in detecting organophosphorus pesticide residues in subsidiary agricultural products.
Description
Technical field
The present invention relates to the detection technique field of pesticide residue, be a kind of inspection with paper battery as power in particular
Survey the preparation of the Electrochemiluminescsensor sensor of organophosphorus pesticide thing.
Background technology
In order to effectively prevent and control disease, worm, grass and other harmful organisms, agriculture and forestry production is worked the mischief, high toxicity
Organophosphorus pesticide is widely used.To a certain extent, the pest and disease damage problem of crops administered effectively by organophosphorus pesticide, gives
Economic results in society bring growth clearly.But, while ensureing that crops are significantly increased production, making of organophosphorus pesticide
The most increasingly highlight with the adverse side effect brought.After organophosphorus pesticide is used, a part is attached to plant surface or oozes
Enter in plant, make grain, vegetable and fruit etc. be contaminated；Another part is then scattered in soil or spills into through pervaporation
In air, or along with agricultural drain and rainwater flow into rivers,lakes and seas, soil, water body and aquatile etc. is made to be contaminated.People master
Pesticide taken in from environment by diet to be passed through.Although the residual concentration that pesticide is in the environment is the highest, but passes through bioconcentration
After the cumulative function of food chain, pesticide concentration can reach thousand of times in vivo, even several ten thousand times.Once organophosphor agriculture
Medicine enters organism, the activity of internal acetylcholine vinegar enzyme will be produced inhibitory action in various degree, even cause disease
And death.Organophosphorus pesticide in food not only affects international trade, more people's health is brought great threat.
Therefore, detection trace organophosphorus pesticide carrying out quickness and high efficiency becomes more and more important.
At present, the main method to trace detection of organic phosphorus pesticide have chromatography and with fourier infrared or mass spectrometry
Technology, these methods are that the mensuration of pesticide residual contamination thing provides effective means.Loaded down with trivial details yet with pre-treatment, equipment is held high
Expensive, the high deficiency of testing cost, these methods are difficult to spread to the analysis testing laboratory of basic unit.Document is had to report employing electricity
The scheme of chemiluminogenic technology for detection organophosphorus pesticide, but the multi-functional electrochemistry of article use and chemiluminescence analysis
Instrument is expensive, can not meet actually detected needs.
Summary of the invention
The technical problem to be solved in the present invention be to provide one have sample treatment be simple and convenient to operate, with low cost etc.
The organophosphorus pesticide object detecting method of feature.
In order to solve above-mentioned technical problem, the present invention is by preparing paper battery, and with preparation paper battery for power structure
Build what the Electrochemiluminescsensor sensor for organophosphorus pesticide analyte detection realized.This detection organophosphorus pesticide thing
The preparation method of sensor be:
(1) CorelDRAW Graphics Suite X6, Adobe Photoshop CS6 or Adobe are used
Illustrator CS6 software design paper battery pattern as shown in Figure 1, paper battery pattern includes filling district, salt bridge district, electrolysis
Matter district, battery area and connecting line district.
(2) filter paper is cut into the size of A4 size, utilizes solid wax printer to be printed by the pattern of design in step (1)
On the filter paper cut out, subsequently the filter paper of printed pattern is placed in heat treated 3 min in the baking oven of 90 DEG C, makes patterning
Wax melts and is formed hydrophobic dam.
(3) using card punch or laser cutting machine to punch between two parties in filling district, bore dia is than reserved hydrophilic area diameter
Little 1 mm；NaCl solution or the KCl solution of 1.0 M is dripped in salt bridge district；0.9 M is dripped respectively in two regions of electrolyte
Cu(NO3)2Solution and 0.6 M Al (NO3)3Solution；At two electrode districts copper foil and aluminium foil respectively；Use in connecting line district
Existing method growth in situ nanometer gold, constructs the gold bonding wire of through paper base material upper and lower surface, then with Achates hammer to paper substrate
The two-sided gold bonding wire of material carries out unidirectional polishing；Filter paper is folded by matter to be electrolysed and saline solution after drying；By dovetail clip
Self-control chip gripper as shown in Figure 2 is fixed.
(4) structure of sensor
It is processed by shot blasting, respectively in ultra-pure water and second with the alumina powder foot couple glass-carbon electrode of 1.0,0.3,0.05 μm successively
Ultrasonic cleaning in alcohol, nitrogen dries up；Glass-carbon electrode after processing inserts in the chlorauric acid solution that mass fraction is 1%, uses electricity
Position stripping analysis technology, the voltage of applying-0.2 V 50 seconds, deposit one layer of gold nano grain at electrode surface；According to existing method
Prepare carbon point as electrogenerated chemiluminescence material；By the carbon point solution drop coating of preparation in the glass-carbon electrode table of gold nano particle modification
Face, is dried；Take 10 microlitre acetylcholinesterase drop coatings electrode surface after modifying, in 4 DEG C of refrigerators, hatch 2 h, use pH
7.4 buffer solution clean；Drip 10 microlitre glutaraldehydes, in 4 DEG C of refrigerators, react 30 min, clean with pH 7.4 buffer solution.
(5) determination step
Sensor prepared by step (4) is placed in the solution containing organophosphorus pesticide thing and reacts 20 min；Then will pass
Sensor is transferred to pH 8.0 containing in the acetyl chloride thiocholine solution of 1.5 mM, with the paper battery of preparation as power, connects
Glass-carbon electrode and Ag/AgCl reference electrode, drip secondary water activated battery in the filling district of paper battery, coordinates stream after stablizing 30 s
Dynamic injected chemical luminescence analyzer detects.
Filling district a diameter of 3-6 mm of the paper battery described in step (1)；Salt bridge sector width is 3-8 mm, a length of
8-20 mm；Electrolyte region a diameter of 3-8 mm；Battery area a diameter of 3-8 mm；Connecting line district a diameter of 3-8 mm.
Self-control chip gripper described in step (3) includes 2, has a hole, the size in hole and filling in the middle of a piece of chip
Hole, district equivalently-sized；There is conductive aluminum circuit on the most a piece of chip gripper, the electric current on connecting line can be drawn.
Paper battery described in step (5) with the connected mode of glass-carbon electrode and reference electrode is, the positive pole of paper battery with
Reference electrode connects, and the negative pole of paper battery is connected with glass-carbon electrode.
Beneficial effects of the present invention
(1) the Electrochemiluminescsensor sensor preparation method being Dynamic testing organophosphorus pesticide thing with paper battery, will design
The paper battery of preparation introduces in detection device as power, reduces testing cost.
(2) this sensor is prepared simply, is easy to carry.
(3) the paper battery preparation method used is simple, and paper base material abundance is collapsible disposable.
(4) nanometer gold using existing method growth in situ to obtain in connecting line district is possible not only to realize the one side of paper base material
Conduction, and because the upper and lower surface of the through paper base material of nanometer gold, it is achieved that the conducting of paper base material upper and lower surface.
Description of drawings 1 is for preparing the hydrophobic wax pattern of paper battery；
The self-control chip gripper that Fig. 2 fixes for paper battery.
Detailed description of the invention
In order to be more fully understood that the present invention, it is further elucidated with present disclosure below in conjunction with embodiment and accompanying drawing, but this
The content of invention is not limited solely to following enforcement.
Embodiment 1. 1 kinds detects the preparation method of the Electrochemiluminescsensor sensor of parathion-methyl pesticide residue
(1) CorelDRAW Graphics Suite X6, Adobe Photoshop CS6 or Adobe are used
Illustrator CS6 software design paper battery pattern as shown in Figure 1, paper battery pattern includes filling district, salt bridge district, electrolysis
Matter district, battery area and connecting line district.
(2) filter paper is cut into the size of A4 size, utilizes solid wax printer to be printed by the pattern of design in step (1)
On the filter paper cut out, subsequently the filter paper of printed pattern is placed in heat treated 3 min in the baking oven of 90 DEG C, makes patterning
Wax melts and is formed hydrophobic dam.
(3) using card punch or laser cutting machine to punch between two parties in filling district, bore dia is than reserved hydrophilic area diameter
Little 1 mm；NaCl solution or the KCl solution of 1.0 M is dripped in salt bridge district；0.9 M is dripped respectively in two regions of electrolyte
Cu(NO3)2Solution and 0.6 M Al (NO3)3Solution；At two electrode districts copper foil and aluminium foil respectively；Use in connecting line district
Existing method growth in situ nanometer gold, constructs the gold bonding wire of through paper base material upper and lower surface, then with Achates hammer to paper substrate
The two-sided gold bonding wire of material carries out unidirectional polishing；Filter paper is folded by matter to be electrolysed and saline solution after drying；By dovetail clip
Self-control chip gripper as shown in Figure 2 is fixed.
(4) structure of sensor
It is processed by shot blasting, respectively in ultra-pure water and second with the alumina powder foot couple glass-carbon electrode of 1.0,0.3,0.05 μm successively
Ultrasonic cleaning in alcohol, nitrogen dries up；Glass-carbon electrode after processing inserts in the chlorauric acid solution that mass fraction is 1%, uses electricity
Position stripping analysis technology, the voltage of applying-0.2V 50 seconds, deposit one layer of gold nano grain at electrode surface；According to existing method
Prepare carbon point as electrogenerated chemiluminescence material；By the carbon point solution drop coating of preparation in the glass-carbon electrode table of gold nano particle modification
Face, is dried；Take 10 microlitre acetylcholinesterase drop coatings electrode surface after modifying, in 4 DEG C of refrigerators, hatch 2 h, use pH
7.4 buffer solution clean；Drip 10 microlitre glutaraldehydes, in 4 DEG C of refrigerators, react 30 min, clean with pH 7.4 buffer solution.
(5) determination step
Sensor prepared by step (4) is placed in the solution containing parathion-methyl residue and reacts 20 min；Then will pass
Sensor is transferred to pH 8.0 containing in the acetyl chloride thiocholine solution of 1.5 mM, with the paper battery of preparation as power, connects
Glass-carbon electrode and Ag/AgCl reference electrode, drip secondary water activated battery in the filling district of paper battery, coordinates stream after stablizing 30 s
Dynamic injected chemical luminescence analyzer detects.
A diameter of 3 mm in filling district of the paper battery described in step (1)；Salt bridge sector width is 3 mm, a length of 8 mm；
A diameter of 3 mm in electrolyte region；A diameter of 3 mm in battery area；A diameter of 3 mm in connecting line district.
Described in step (3) self-control chip gripper include 2, have a hole, the size in hole in the middle of the most a piece of chip
With filling hole, district equivalently-sized；There is conductive aluminum circuit on the most a piece of chip gripper, the electric current on connecting line can be drawn.
Paper battery described in step (5) with the connected mode of glass-carbon electrode and reference motor is, the positive pole of paper battery with
Reference electrode connects, and the negative pole of paper battery is connected with glass-carbon electrode.
Embodiment 2. 1 kinds detects the preparation method of the Electrochemiluminescsensor sensor of demeton pesticide residue
Preparation process, with example 1, is a difference in that:
A diameter of 5 mm in filling district of the paper battery described in step (1)；Salt bridge sector width is 5 mm, a length of 12 mm；Electricity
A diameter of 5 mm in Xie Zhi district；A diameter of 5 mm in battery area；A diameter of 5 mm in connecting line district.
Described in step (3) self-control chip gripper include 2, have a hole, the size in hole in the middle of the most a piece of chip
With filling hole, district equivalently-sized；There is conductive aluminum circuit on the most a piece of chip gripper, the electric current on connecting line can be drawn.
Organophosphorus pesticide in step (5) is demeton pesticide.
Embodiment 3. 1 kinds detects the preparation method of the Electrochemiluminescsensor sensor of Malathion pesticide residue
Preparation process, with example 1, is a difference in that:
A diameter of 6 mm in filling district of the paper battery described in step (1)；Salt bridge sector width is 8 mm, a length of 16 mm；Electricity
A diameter of 8.0 mm in Xie Zhi district；A diameter of 8 mm in battery area；A diameter of 8 mm in connecting line district.
Described in step (3) self-control chip gripper include 2, have a hole, the size in hole in the middle of the most a piece of chip
With filling hole, district equivalently-sized；There is conductive aluminum circuit on the most a piece of chip gripper, the electric current on connecting line can be drawn.
Organophosphorus pesticide in step (5) is Malathion pesticide.
Claims (4)
1. the preparation method of the Electrochemiluminescsensor sensor detecting organophosphorus pesticide thing, it is characterised in that preparation step
Rapid as follows:
(1.1) CorelDRAW Graphics Suite X6, Adobe Photoshop CS6 or Adobe are used
Illustrator CS6 software design paper battery pattern, paper battery pattern includes filling district, salt bridge district, electrolyte region, battery area
With connecting line district；
(1.2) filter paper is cut into the size of A4 size, utilizes solid wax printer to be printed by the pattern of design in step (1.1)
On the filter paper cut out, subsequently the filter paper of printed pattern is placed in heat treated 3 min in the baking oven of 90 DEG C, makes patterning
Wax melts and is formed hydrophobic dam；
(1.3) using card punch or laser cutting machine to punch between two parties in filling district, bore dia is less by 1 than reserved hydrophilic area diameter
mm；NaCl solution or the KCl solution of 1.0 M is dripped in salt bridge district；0.9 M Cu is dripped respectively in two regions of electrolyte
(NO3)2Solution and 0.6 M Al (NO3)3Solution；At two electrode districts copper foil and aluminium foil respectively；Use existing in connecting line district
There is method growth in situ nanometer gold, construct the gold bonding wire of through paper base material upper and lower surface, then with Achates hammer to paper base material
Two-sided gold bonding wire carries out unidirectional polishing；Filter paper is folded by matter to be electrolysed and saline solution after drying；By dovetail clip and
Self-control chip gripper is fixed；
(1.4) structure of sensor
It is processed by shot blasting, respectively in ultra-pure water and second with the alumina powder foot couple glass-carbon electrode of 1.0,0.3,0.05 μm successively
Ultrasonic cleaning in alcohol, nitrogen dries up；Glass-carbon electrode after processing inserts in the chlorauric acid solution that mass fraction is 1%, uses electricity
Position stripping analysis technology, the voltage of applying-0.2 V 50 seconds, deposit one layer of gold nano grain at electrode surface；According to existing method
Prepare carbon point as electrogenerated chemiluminescence material；By the carbon point solution drop coating of preparation in the glass-carbon electrode table of gold nano particle modification
Face, is dried；Take 10 microlitre acetylcholinesterase drop coatings electrode surface after modifying, in 4 DEG C of refrigerators, hatch 2 h, use pH
7.4 buffer solution clean；Drip 10 microlitre glutaraldehydes, in 4 DEG C of refrigerators, react 30 min, clean with pH 7.4 buffer solution；
(1.5) determination step
Sensor prepared by step (1.4) is placed in the solution containing organophosphorus pesticide thing and reacts 20 min；Then will
Sensor is transferred to pH 8.0 containing in the acetyl chloride thiocholine solution of 1.5 mM, with the paper battery of preparation as power, even
Connect glass-carbon electrode and Ag/AgCl reference electrode, drip secondary water activated battery in the filling district of paper battery, coordinate after stablizing 30 s
Flow Injection Analysis/Chemiluminescence instrument detects.
The preparation side of a kind of Electrochemiluminescsensor sensor detecting organophosphorus pesticide thing the most as claimed in claim 1
Method, is characterized in that filling district a diameter of 3-6 mm of the paper battery described in step (1.1)；Salt bridge sector width is 3-8 mm, long
Degree is 8-20 mm；Electrolyte region a diameter of 3-8 mm；Battery area a diameter of 3-8 mm；Connecting line district a diameter of 3-8 mm.
The preparation side of a kind of Electrochemiluminescsensor sensor detecting organophosphorus pesticide thing the most as claimed in claim 1
Method, it is characterized in that the self-control chip gripper described in step (1.3) includes 2, has a hole in the middle of the most a piece of chip, hole
Size is equivalently-sized with filling hole, district；There is conductive aluminum circuit on the most a piece of chip gripper, the electric current on connecting line can be drawn
Go out.
The preparation side of a kind of Electrochemiluminescsensor sensor detecting organophosphorus pesticide thing the most as claimed in claim 1
Method, is characterized in that the paper battery described in step (1.5) is that paper battery is just with the connected mode of glass-carbon electrode and reference motor
Pole is connected with reference electrode, and the negative pole of paper battery is connected with glass-carbon electrode.
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|---|---|---|---|
| CN201610650613.9A CN106323950B (en) | 2016-08-10 | 2016-08-10 | A kind of preparation method of the sensor of detection organophosphorus pesticide object |
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| CN201610650613.9A CN106323950B (en) | 2016-08-10 | 2016-08-10 | A kind of preparation method of the sensor of detection organophosphorus pesticide object |
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| CN106323950A true CN106323950A (en) | 2017-01-11 |
| CN106323950B CN106323950B (en) | 2018-09-07 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108613954A (en) * | 2018-04-27 | 2018-10-02 | 重庆大学 | A kind of detection method of carbendazim |
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| CN108613954B (en) * | 2018-04-27 | 2020-11-24 | 重庆大学 | Detection method of carbendazim |
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| CN106323950B (en) | 2018-09-07 |
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