CN109975281A - A kind of method for preparing test paper detecting organophosphorus pesticide - Google Patents
A kind of method for preparing test paper detecting organophosphorus pesticide Download PDFInfo
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- CN109975281A CN109975281A CN201910227758.1A CN201910227758A CN109975281A CN 109975281 A CN109975281 A CN 109975281A CN 201910227758 A CN201910227758 A CN 201910227758A CN 109975281 A CN109975281 A CN 109975281A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
- B32B27/304—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising vinyl halide (co)polymers, e.g. PVC, PVDC, PVF, PVDF
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
- B32B27/322—Layered products comprising a layer of synthetic resin comprising polyolefins comprising halogenated polyolefins, e.g. PTFE
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B29/00—Layered products comprising a layer of paper or cardboard
- B32B29/002—Layered products comprising a layer of paper or cardboard as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B29/00—Layered products comprising a layer of paper or cardboard
- B32B29/002—Layered products comprising a layer of paper or cardboard as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B29/005—Layered products comprising a layer of paper or cardboard as the main or only constituent of a layer, which is next to another layer of the same or of a different material next to another layer of paper or cardboard layer
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- G—PHYSICS
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- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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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
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N2021/7756—Sensor type
- G01N2021/7759—Dipstick; Test strip
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Abstract
The present invention relates to a kind of test paper of quickly detection organophosphorus pesticide: utilizing MULTILAYER COMPOSITE means, it allows containing organic phosphorus prepare liquid respectively by being fixed with different reagents, upper, middle and lower-ranking filter paper with different function realizes the purpose that organophosphorus pesticide is quickly detected using development process.Every layer of filter paper first printed pool using wax spray printer and the area that blocks water, then on upper layer, filter paper is crossed and fixes hydrophobic adsorbent material in pool respectively, filter paper, which is crossed, in middle level fixes buffer salt in pool, it is crossed in pool in lower layer's filter paper and fixes redox color developing agent, and be close to thin film in lower layer's filter paper bottom.It is organic phosphorus to be adsorbed during permeating upper layer by hydrophobicity, continuous enrichment method is in the filter paper of upper layer, then pass through alkaline hydrolysis, by buffer salt fixed in middle layer, after having adjusted pH value, into lower layer, by the oxidizing of lower layer, oxidant generates color change after being reduced, and determines whether that there are organophosphorus pesticides by color change.
Description
Technical field
The present invention relates to it is a kind of utilize MULTILAYER COMPOSITE means, by three layers be respectively provided with enrichment, buffering, coloring function filter paper
Superposition prepares the method that can quickly detect organophosphorus pesticide test paper.
Background technique
Organophosphorus pesticide refers to the organic compound pesticide of phosphorus element-containing, mostly phosphoric acid ester or group thiophosphate, tool
Have the advantages that wide spectrum, efficiently, the mode of action mostly and half-life short, be widely used in agricultural production.But chronic administration such
Different degrees of residual can not only occur in crops for pesticide, can also contaminated soil, water and air, cause serious environment
Problem threatens the health of the mankind.Technology about residues of organophosphate pesticides detection has research more, and existing detection means includes chromatography
Method (such as gas-chromatography, high performance liquid chromatography, gas chromatography mass spectrometry, LC-MS etc.), spectroscopic methodology, hexavalent chrome bio-removal, enzyme linked immunological
Method, molecular imprinting method, and the enzyme inhibition generallyd use in organic phosphorus fast inspection field.
The basic principle of enzyme inhibition is to utilize enzyme to the active inhibiting effect of enzyme acetylcholine according to organophosphorus insecticide
The chromogenic reaction occurred with substrate is measured enzyme inhibition rate, and then realizes the quantitative analysis of organophosphorus pesticide.It is main excellent
Point is that cost is relatively low, sensitivity is higher, easy to operate.Enzymatic test paper based on enzyme inhibition exploitation is the residual detection of agriculture not against instrument
But there is enzymatic reaction to temperature requirement height, need at 37 degrees Celsius of constant temperature 3-5 points in device, the main means that the scene of realization is examined fastly
Clock is not easy the problem of realizing in actual operation.
After organic phosphorus hydrolysis under alkaline condition, the hydrolysate with reproducibility is generated, when itself and oxidant such as Gao Meng
After sour potassium or iron chloride reaction, oxidant can be made to generate color change, variation degree with colorimetric card by compareing, it is possible to determine that has
The content of machine phosphorus provides feasibility foundation for the test paper technology of preparing of this detection organophosphorus pesticide.
Summary of the invention
The technical problem to be solved by the present invention is to be based on chromogenic reaction, using the means of MULTILAYER COMPOSITE test paper, realize organic
The purpose that the residual scene of phosphorus agriculture is examined fastly.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of method for preparing test paper detecting organophosphorus pesticide, it is characterised in that follow the steps below: test paper is divided into
Upper, middle and lower-ranking printed pool by wax spray printer and blocked water area, wherein upper layer test paper cross pool be fixed with it is thin
Aqueous adsorbent material, middle layer filter paper cross pool and are fixed with buffer salt, and lower layer's filter paper crosses pool and is fixed with redox color developing agent, and
Being close to thin film in lower layer's filter paper bottom prevents fluid seepage.When being detected to sample to be tested, prepare liquid is dripped to first
Upper layer is crossed on pool, and pads water-absorbent material in lower section, makes organic phosphorus solution quilt during flowing through hydrophobic adsorbent material
Continuous enrichment method later removes the water-absorbent material below filter paper, and upper layer and middle layer, lower layer are attached onto, and makes hydrophilic
Area is overlapped, forms three-layer composite structure.Later upper layer be added dropwise strong base solution, it is organic phosphorus hydrolyzed by strong base solution after, from
It is eluted out in silica gel adsorptive material, into middle layer buffer salt area, after having adjusted pH value, infiltrates through lower layer, the oxygen with lower layer
Redox reaction occurs for agent, and oxidant generates color change after being reduced, and lower layer's filter paper is removed, by determining oxidant
Color change intensity is realized to organic phosphorus qualitative and quantitative analysis.
The organophosphorus pesticide include DDVP, Rogor, metrifonate, phoxim, parathion, flolimat, acephatemet,
Chlopyrifos, orthene, malathion, Hostathion, fenifrothion, glyphosate, tolelofos-methyl, kitazine, metrifonate, third
The phonetic phosphorus of bromine phosphorus, methidathion, An Guo, Entex, phenothiazide, pyrrole, phenthoate dimephenthoate cidial, dioxathion edifenphos, diazinon, metilomerkaptofosoksid, volt kill
Sulphur phosphorus, thimet, chlorpyrifos-methyl, parathion-methyl, methyl azinphos-methyl, ethoprop, Afos, Nankor, isocarbophos, first
Yl pyrimidines phosphorus, demeton-methyl, Isofenphos methyl, Azodrin, quinalphos, phosphamidon cadusafos, terbufos, the complete sulphur phosphorus, Asia of going out
Amine sulphur phosphorus, disulfoton, ethyl Gu sulphur phosphorus, Rilariol, ethephon (CEPHA),2-(chloroethyl) phosphonic acid, cynock, salithion, sulfotep, first Toyodan, pyridazine
Sulphur phosphorus, Phosalone, Menite, Fonofos, tolelofos-methyl, phosfolan, isazofos, lythidathion, Ethodan, different rice blast
Only, Terbufos, phosfolan, Folithion, cynock, salithion, Resistox, sulfotep, first Toyodan, pyridaphethione, volt kill sulphur
One or more of phosphorus, Toyodan, demeton.
Described crosses the circle that pool is 1~10mm of diameter, the preferably circle of 1~7mm, the preferably circle of 2~4mm.Diameter
Too small, the surface tension of solution causes water droplet to float on the wax to block water, and water speed is extremely slow excessively or is difficult to water；Diameter is excessive, molten
Liquid does not come also anxious to be diffused into round edge and just flow through from center, it is difficult to form uniform color change.
It by wax that wax melts is 50~60 μm of drop forms according to design with diameter that the area that blocks water, which is by wax spray printing,
On pattern surface to filter paper, and quick solidification, it is then heated 0.5~10 minute by 80~150 degree in baking oven, keeps wax complete
Melt and penetrate into filter paper fibre entirely and is formed.
The hydrophobic adsorbent material is hydrophobic silicone, 300~800m of specific surface area2/ g, 10~60 μm of partial size dredge
One or both of aqueous silica sol particle or C18 adsorbent material octadecylsilane chemically bonded silica filler C18, fixed amount are
10~20mg/cm2。
The water-absorbent material is one of absorbent wool, macromolecule water uptake polymer, filter paper.
The strong base solution be one of the sodium hydroxide of 0.5~1.0M, potassium hydroxide, sodium ethoxide, ammonium hydroxide or
Two or more several, usage amount is 0.2~0.5mL.
The buffer salt area is the pH tune of 0.02~0.2M of 200~300 μ L of drop coating on the hydrophilic area of middle layer test paper
Buffer of the energy saving power between 6.0~7.5, including citric acid-sodium citrate, disodium hydrogen phosphate-sodium dihydrogen phosphate, phosphoric acid hydrogen
One or more of disodium-potassium dihydrogen phosphate, potassium dihydrogen phosphate-sodium hydroxide system is two or more, dries spare.
The redox color developing agent is potassium permanganate or iron chloride, and the fixed amount on hydrophilic area is 0.1~1.0mg/
cm2。
The film is one of PET, PTFE, PVC film.
Detection process is as follows: taking 500 μ L solution to be measured to be added drop-wise on the filter paper of upper layer, is absorbed to solution by lower section water-absorbent material
Afterwards, water-absorbent material is removed, by upper layer filter paper and middle lower layer's filter paper overlaid, so that hydrophilic area overlaps each other, on the filter paper stacked
Lye is added dropwise, stands 5 minutes, removes upper middle layer filter paper, lower layer's filter paper indicator color change is observed, to judge solution to be measured
Whether organophosphorus insecticide is contained.The immobilized test paper for having potassium permanganate, if organophosphorus insecticide exist, test paper color from red to
It is pale red to yellow change；The immobilized test paper for having iron chloride, if organophosphorus insecticide exists, test paper color is from yellow to pale yellow to white
Color change.
The present invention has the advantage that
1. by the utilization of hydrophobic adsorbent material, by fruit and vegetable eluent it is hydrophobic it is organic phosphorus adsorb, keep away
The use of cumbersome sample pretreatment process and toxic organic solvents is exempted from；
2. being completed in organic phosphorus basic hydrolysis and buffering and in test paper previous step, reduces to react in solution acid solution is added dropwise again
The trouble of neutralization；
3. entire organic phosphorus detection is completed by three layers of test paper superposition of upper, middle and lower, easy to operation；
4. test paper of the present invention is cheap, environmental-friendly, it is suitable for field quick detection.
Detailed description of the invention
Fig. 1 is the test paper schematic diagram for detecting organophosphorus pesticide.
Fig. 2 is using potassium permanganate as the organic phosphorus Test paper response diagram of oxidant
A) figure that potassium permanganate original image b) potassium permanganate is reduced.
Fig. 3 is using iron chloride as the organic phosphorus Test paper response diagram of oxidant.
A) figure that iron chloride original image b) iron chloride is reduced
Fig. 4 is to detect organophosphorus pesticide test paper to the response diagram of various concentration Rogor.
Fig. 5 is to detect organophosphorus pesticide test paper (potassium permanganate) to the linear response curve of various concentration Rogor.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as this hair
Bright to be limited only to following embodiment, all technologies realized based on the content of present invention are regarded as the scope of the present invention.
Embodiment 1
By three 2x2cm2Filter paper by coating of wax on wax spray printer surface, there are the skies of diameter 3mm at center
White circle crosses pool, and the filter paper of waxing is placed in baking oven and is dried 2 minutes for 150 degree, so that wax uniformly melts and penetrates into filter paper
In fiber, the area that blocks water is formed.The evenly dispersed C18 powder of ethyl alcohol, fixed amount 10mg/ is added dropwise in crossing on pool for upper layer filter paper
cm2, dry up spare；The 250 μ L of sodium dihydrogen phosphate-disodium hydrogen phosphate buffer for crossing pool and 0.025M being added dropwise of filter paper in middle level,
It dries up spare；In the liquor potassic permanganate of lower layer's filter paper crossed pool and 35 microlitres of 1g/L are added dropwise, it is made to fix 0.5mg/cm2Height
Potassium manganate, drying is spare, and lower layer's filter paper bottom is stained with PET film, as shown in Figure 1.
The epidermis of pears is cleaned with clear water, Rogor standard sample is added dropwise in the cleaning solution, reaches its concentration about
1ppm.500 μ L of the mark-on solution is added dropwise dropwise in the pool of crossing of upper layer filter paper, upper water-absorbent material is padded in decentralization, all flows to solution
After crossing upper layer filter paper, by upper layer filter paper and middle lower layer's filter paper overlaid, 50 μ L of 1.0M NaOH solution is added dropwise, stands 5 minutes, removes
Upper middle layer filter paper, as shown in Figure 2, it is seen that significant change occurs for the potassium permanganate color that lower layer's filter paper crosses pool, becomes from red
Yellow, it may be verified that in the pears sample of mark-on Rogor there are organophosphorus pesticides.
Embodiment 2
By three 2x2cm2Filter paper by coating of wax on wax spray printer surface, there are the skies of diameter 3mm at center
White circle crosses pool, and the filter paper of waxing is placed in baking oven and is dried 10 minutes for 90 degree, so that wax uniformly melts and penetrates into filter paper
In fiber, the area that blocks water is formed.The evenly dispersed dewatering silica gel particle of ethyl alcohol is added dropwise in crossing on pool for upper layer filter paper, fixed amount is
20mg/cm2, dry up spare；The 250 μ L of citric acid-sodium citrate buffer for crossing pool and 0.2M being added dropwise of filter paper in middle level, blows
It does spare；In the iron chloride of lower layer's filter paper crossing pool and being added dropwise, the ferric chloride solution of 35 microlitres of 2g/L is added dropwise, makes its fixed amount
1mg/cm2, drying is spare, and lower layer's filter paper bottom is stained with PET film, as shown in Figure 1.
The epidermis of Chinese cabbage is cleaned with clear water, metrifonate standard sample is added dropwise in the cleaning solution, reaches its concentration
About 1ppm.500 μ L of the mark-on solution is added dropwise dropwise in the pool of crossing of upper layer filter paper, upper water-absorbent material is padded in decentralization, to solution whole
After flowing through upper layer filter paper, by upper layer filter paper and middle lower layer's filter paper overlaid, 100 μ L of 0.8M KOH solution is added dropwise, stands 5 minutes, goes
Fall upper middle layer filter paper, it is seen that significant change occurs for the iron chloride color that lower layer's filter paper crosses pool, and test paper becomes white by yellow,
As shown in Figure 3, it may be verified that contain organophosphorus insecticide in the Chinese cabbage sample of mark-on metrifonate.
Embodiment 3
By three 2x2cm2Filter paper by coating of wax on wax spray printer surface, there are the skies of diameter 3mm at center
White circle crosses pool, and the filter paper of waxing is placed in baking oven and is dried 2 minutes for 150 degree, so that wax uniformly melts and penetrates into filter paper
In fiber, the area that blocks water is formed.The evenly dispersed C18 powder of ethyl alcohol, fixed amount 15mg/ is added dropwise in crossing on pool for upper layer filter paper
cm2, dry up spare；The sodium dihydrogen phosphate for crossing pool dropwise addition 0.025M-disodium hydrogen phosphate buffer buffering of filter paper is molten in middle level
250 μ L of liquid is dried up spare；Potassium permanganate is added dropwise in the pool of crossing of lower layer's filter paper, the liquor potassic permanganate of 35 microlitres of 1g/L is added dropwise,
Make its fixed amount 0.5mg/cm2, drying is spare, and lower layer's filter paper bottom is stained with PET film.
The epidermis of tomato is cleaned with clear water, Rogor standard sample is added dropwise in the cleaning solution, distinguishes its concentration
Reach about 0.5,1,1.5,2,2.5ppm, 500 μ L of the mark-on solution is added dropwise dropwise respectively in the pool of crossing of upper layer filter paper, decentralization pad
After solution all flows through upper layer filter paper, by upper layer filter paper and middle lower layer's filter paper overlaid, 1.0M NaOH is added dropwise in upper water-absorbent material
50 μ L of solution stands 5 minutes, removes upper middle layer filter paper, it is seen that lower layer's filter paper crosses the potassium permanganate color in pool with mark-on agriculture
The increase of medicine Rogor concentration and gradually change, yellow is gradually transformed by red, as shown in Figure 4.By each of which concentration pair
The potassium permanganate color value (square in three channels of RGB) and Rogor concentration answered do curve, and preferable correlation can be obtained and close
System, as shown in Figure 5, it may be verified that contain organophosphorus insecticide, and test paper color change intensity in the tomato sample of mark-on Rogor
Increase with the increase of organophosphorus pesticide concentration, when mark-on Rogor concentration reaches 0.8ppm, color change tends to be saturated, and says
Bright test paper of the present invention, which has the organophosphorus pesticide of low concentration, preferably responds the half-quantitative detection, it can be achieved that low concentration pesticide.
Embodiment 4
By three 2x2cm2Filter paper by coating of wax on wax spray printer surface, there are the skies of diameter 3mm at center
White circle crosses pool, and the filter paper of waxing is placed in baking oven and is dried 8 minutes for 110 degree, so that wax uniformly melts and penetrates into filter paper
In fiber, the area that blocks water is formed.It is in the dewatering silica gel particle fixed amount that dropwise addition ethyl alcohol is evenly dispersed on pool of crossing of upper layer filter paper
18mg/cm2, dry up spare；The 250 μ L of citric acid-sodium citrate buffer for crossing pool and 0.2M being added dropwise of filter paper in middle level, blows
It does spare；Ferric chloride in aqueous solution is added dropwise in the pool of crossing of lower layer's filter paper, the ferric chloride solution of 28 microlitres of 2g/L is added dropwise, forms it into
Supported quantity is 0.8mg/cm2Test paper, dry up it is spare, lower layer's filter paper bottom is stained with PET film.
The epidermis of peach is cleaned with clear water, metrifonate standard sample is added dropwise in the cleaning solution, reaches its concentration
About 1ppm.500 μ L of the mark-on solution is added dropwise dropwise in the pool of crossing of upper layer filter paper, upper water-absorbent material is padded in decentralization, to solution whole
After flowing through upper layer filter paper, by upper layer filter paper and middle lower layer's filter paper overlaid, 100 μ L of 0.8M KOH solution is added dropwise, stands 5 minutes, goes
Fall upper middle layer filter paper, it is seen that significant change occurs for the iron chloride color that lower layer's filter paper crosses pool, becomes faint yellow from yellow.
Embodiment 5
By three 2x2cm2Filter paper by coating of wax on wax spray printer surface, there are the skies of diameter 3mm at center
White circle crosses pool, and the filter paper of waxing is placed in baking oven and is dried 2 minutes for 150 degree, so that wax uniformly melts and penetrates into filter paper
In fiber, the area that blocks water is formed.The evenly dispersed C18 powder of ethyl alcohol, fixed amount 10mg/ is added dropwise in crossing on pool for upper layer filter paper
cm2, dry up spare；The 250 μ L of sodium dihydrogen phosphate-disodium hydrogen phosphate buffer for crossing pool and 0.025M being added dropwise of filter paper in middle level,
It dries up spare；In the liquor potassic permanganate of lower layer's filter paper crossed pool and 35 microlitres of 1g/L are added dropwise, it is made to fix 0.5mg/cm2Height
Potassium manganate, drying is spare, and lower layer's filter paper bottom is stained with PET film, as shown in Figure 1.
Celery is cleaned with clear water, metrifonate standard sample is added dropwise in the cleaning solution, its concentration is made to reach about 1ppm.
500 μ L of the mark-on solution is added dropwise dropwise in the pool of crossing of upper layer filter paper, decentralization pads upper water-absorbent material, all flows through upper layer to solution
After filter paper, by upper layer filter paper and middle lower layer's filter paper overlaid, 50 μ L of 1.0M NaOH solution is added dropwise, stands 5 minutes, removes upper middle layer
Filter paper, it is seen that significant change occurs for the potassium permanganate color that lower layer's filter paper crosses pool, becomes yellow from red.
Embodiment 6
By three 2x2cm2Filter paper by coating of wax on wax spray printer surface, there are the skies of diameter 3mm at center
White circle crosses pool, and the filter paper of waxing is placed in baking oven and is dried 2 minutes for 150 degree, so that wax uniformly melts and penetrates into filter paper
In fiber, the area that blocks water is formed.The evenly dispersed C18 powder of ethyl alcohol, fixed amount 15mg/ is added dropwise in crossing on pool for upper layer filter paper
cm2, dry up spare；The sodium dihydrogen phosphate for crossing pool dropwise addition 0.025M-disodium hydrogen phosphate buffer buffering of filter paper is molten in middle level
250 μ L of liquid is dried up spare；Potassium permanganate is added dropwise in the pool of crossing of lower layer's filter paper, the liquor potassic permanganate of 35 microlitres of 1g/L is added dropwise,
Make its fixed amount 0.5mg/cm2, drying is spare, and lower layer's filter paper bottom is stained with PET film.
Western Lan Huayong clear water is cleaned, thimet standard sample is added dropwise in the cleaning solution, respectively reaches its concentration
About 0.5,1,1.5,2,2.5ppm are added dropwise 500 μ L of the mark-on solution dropwise respectively and inhale on the pool of crossing of upper layer filter paper, decentralization pad
After solution all flows through upper layer filter paper, by upper layer filter paper and middle lower layer's filter paper overlaid, 1.0M NaOH solution is added dropwise in water material
50 μ L stand 5 minutes, remove upper middle layer filter paper, it is seen that lower layer's filter paper crosses the potassium permanganate color in pool as mark-on pesticide is happy
The increase of fruit concentration and gradually change, yellow is gradually transformed by red.
Embodiment 7
By three 2x2cm2Filter paper by coating of wax on wax spray printer surface, there are the skies of diameter 3mm at center
White circle crosses pool, and the filter paper of waxing is placed in baking oven and is dried 8 minutes for 110 degree, so that wax uniformly melts and penetrates into filter paper
In fiber, the area that blocks water is formed.It is in the dewatering silica gel particle fixed amount that dropwise addition ethyl alcohol is evenly dispersed on pool of crossing of upper layer filter paper
18mg/cm2, dry up spare；The 250 μ L of citric acid-sodium citrate buffer for crossing pool and 0.2M being added dropwise of filter paper in middle level, blows
It does spare；Ferric chloride in aqueous solution is added dropwise in the pool of crossing of lower layer's filter paper, the ferric chloride solution of 28 microlitres of 2g/L is added dropwise, forms it into
Supported quantity is 0.8mg/cm2Test paper, dry up it is spare, lower layer's filter paper bottom is stained with PET film.
The epidermis of strawberry is cleaned with clear water, phoxim standard sample is added dropwise in the cleaning solution, reaches its concentration
About 1ppm.500 μ L of the mark-on solution is added dropwise dropwise in the pool of crossing of upper layer filter paper, upper water-absorbent material is padded in decentralization, to solution whole
After flowing through upper layer filter paper, by upper layer filter paper and middle lower layer's filter paper overlaid, 100 μ L of 0.8M KOH solution is added dropwise, stands 5 minutes, goes
Fall upper middle layer filter paper, it is seen that significant change occurs for the iron chloride color that lower layer's filter paper crosses pool, becomes faint yellow from yellow.
Claims (10)
1. a kind of test paper for detecting organophosphorus pesticide, it is characterised in that: Test paper includes upper, middle and lower-ranking filter paper, three layers of filter
Be respectively provided on paper be soaked with wax annular block water area and by ring-type block water area it is circular cross pool；In upper layer, filter paper crosses pool
Fixed (or can be referred to as immobilized or attachment) has a hydrophobic adsorbent material, and middle layer filter paper crosses that pool fixes (or can be referred to as immobilized
Or attachment) there is a buffer salt, lower layer's filter paper, which crosses pool and fixes (or can be referred to as immobilized or attachment), redox color developing agent, upper,
In, lower three layers of test paper cross pool be corresponding in turn to from top to bottom sequence be arranged.
2. the test paper of detection organophosphorus pesticide according to claim 1, it is characterised in that:
Being close to (or attachment) thin film immediately below lower layer's filter paper bottom (or lower part) prevents fluid seepage；The film is
One of PET, PTFE, PVC film.
3. the test paper of detection organophosphorus pesticide according to claim 1, it is characterised in that: the hydrophobic adsorbent material is
300~800m of specific surface area2/ g, 10~60 μm of partial size of hydrophobic silicone particle or octadecylsilane chemically bonded silica filler
One of C18 or two kinds, it is 10~20mg/cm that in upper layer, filter paper, which crosses the fixed amount in pool,2；
The redox color developing agent be potassium permanganate or iron chloride, in lower layer's filter paper cross the fixed amount on pool be 0.1~
1.0mg/cm2。
4. the test paper of detection organophosphorus pesticide according to claim 1, it is characterised in that: buffer salt includes citric acid-lemon
Lemon acid sodium, disodium hydrogen phosphate-sodium dihydrogen phosphate, disodium hydrogen phosphate-potassium dihydrogen phosphate, potassium dihydrogen phosphate-sodium hydroxide buffer body
One or more of buffer salt combination that system uses；
The pH that the buffer salt area is 0.02~0.2M of 200~300 μ L of drop coating on the hydrophilic area of middle layer test paper adjusts energy
Power combines manufactured buffer using above-mentioned buffer salt between 6.0~7.5, dries spare.
5. according to claim 1, detecting the test paper of organophosphorus pesticide described in 3 or 4, it is characterised in that: the pool of crossing is straight
The circle of 1~10mm of diameter, the preferably circle of 1~7mm of diameter, the preferably circle of 2~4mm of diameter.
6. a kind of preparation method of the test paper of any detection organophosphorus pesticide of claim 1-5, it is characterised in that:
It follows the steps below:
1) print the area that blocks water by wax spray printer respectively in three floor test paper: the area that blocks water is that will be melted by wax spray printing
The wax of change is 50~60 μm of drop forms according on required annular patterns surface to filter paper with diameter, wax quick solidification, so
It is heated 0.5~10 minute by 80~150 degree in baking oven afterwards, so that wax is melted completely and is penetrated into filter paper fibre and formed；And shape
At the excessively pool circular by the cyclic annular area that blocks water；
2) in upper layer, filter paper crosses pool and is fixed with hydrophobic adsorbent material, and middle layer filter paper crosses pool and is fixed with buffer salt, lower layer's filter
Paper crosses pool and is fixed with redox color developing agent；
It is filled out in the hydrophobic silicone particle or octadecylsilane chemically bonded silica for crossing dropwise addition ethyl alcohol dispersion on pool of upper layer filter paper
Expect C18, dries up spare；
Buffer is added dropwise in the pool of crossing of filter paper in middle level, dries up spare；
The fixed liquor potassic permanganate in pool or iron oxide solution are crossed in lower layer's filter paper, is dried up spare.
7. detecting the preparation method of the test paper of organophosphorus pesticide according to claim 6, it is characterised in that: lower layer's filter paper bottom
One layer of adherency prevents fluid seepage film.
8. a kind of application of the test paper of any detection organophosphorus pesticide of claim 1-5, it is characterised in that: for organic phosphorus
The detection of pesticide；
The organophosphorus pesticide includes DDVP, Rogor, metrifonate, phoxim, parathion, flolimat, acephatemet, poisons with poison
Tick, orthene, malathion, Hostathion, fenifrothion, glyphosate, tolelofos-methyl, kitazine, metrifonate, the third bromine
The phonetic phosphorus of phosphorus, methidathion, An Guo, Entex, phenothiazide, pyrrole, phenthoate dimephenthoate cidial, dioxathion edifenphos, diazinon, metilomerkaptofosoksid, volt kill sulphur
Phosphorus, thimet, chlorpyrifos-methyl, parathion-methyl, methyl azinphos-methyl, ethoprop, Afos, Nankor, isocarbophos, methyl
Diothyl, demeton-methyl, Isofenphos methyl, Azodrin, quinalphos, phosphamidon cadusafos, terbufos, the complete sulphur phosphorus, imines of going out
Sulphur phosphorus, disulfoton, ethyl Gu sulphur phosphorus, Rilariol, ethephon (CEPHA),2-(chloroethyl) phosphonic acid, cynock, salithion, sulfotep, first Toyodan, pyridazine sulphur
Phosphorus, Phosalone, Menite, Fonofos, tolelofos-methyl, phosfolan, isazofos, lythidathion, Ethodan, different rice blast net,
Terbufos, phosfolan, Folithion, cynock, salithion, Resistox, sulfotep, first Toyodan, pyridaphethione, Phosalone,
One or more of Toyodan, demeton.
9. detecting the application of the test paper of organophosphorus pesticide according to claim 8, it is characterised in that: detection process is as follows,
When being detected to sample to be tested, sample to be tested solution is dripped on the pool excessively of upper layer test paper first, and is tried on upper layer
Water-absorbent material is padded below paper, makes solution during flowing through hydrophobic adsorbent material by continuous enrichment method, later by filter paper
The water-absorbent material of lower section removes；
Upper layer and middle layer, lower layer are successively attached onto, the composite construction of trilaminate stack is formed, makes upper, middle and lower-ranking test paper
Pool of crossing be corresponding in turn to be stacked from top to bottom；On upper layer, test paper is crossed and strong base solution is added dropwise on pool later, organic phosphorus quilt
After strong base solution hydrolysis, it is eluted out from silica gel adsorptive material, into middle layer buffer salt area, after having adjusted pH value, infiltration
Enter lower layer, redox reaction occurs with the oxidant of lower layer, oxidant generates color change, the filter of removing lower layer after being reduced
Paper, by determining that the color change intensity of oxidant is realized to organic phosphorus qualitative and quantitative analysis；
The immobilized test paper for having potassium permanganate, if organophosphorus insecticide exists, with the increase test paper face of organophosphorus insecticide content
Color is from red to pale red to yellow variation；The immobilized test paper for having iron chloride, if organophosphorus insecticide exists, with organic phosphates agriculture
The increase test paper color of medicine content changes from yellow to pale yellow to white.
10. the application of the test paper of detection organophosphorus pesticide according to claim 9, it is characterised in that: the water-absorbent material
For one or more of absorbent wool, macromolecule water uptake polymer, filter paper；
The strong base solution is one or both of the sodium hydroxide of 0.5~1.0M, potassium hydroxide, sodium ethoxide, ammonium hydroxide
More than, usage amount is 50~100 μ L.
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