CN106226292A - The fast of a kind of cyano-containing pyrethroid pesticide examines card and preparation and application - Google Patents
The fast of a kind of cyano-containing pyrethroid pesticide examines card and preparation and application Download PDFInfo
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- CN106226292A CN106226292A CN201610251288.9A CN201610251288A CN106226292A CN 106226292 A CN106226292 A CN 106226292A CN 201610251288 A CN201610251288 A CN 201610251288A CN 106226292 A CN106226292 A CN 106226292A
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- G—PHYSICS
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- 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
- 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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Abstract
The present invention relates to a kind of cyano-containing pyrethroid pesticide examines card soon.This examines the principle of the chemically based colour developing of card soon, after alkaline hydrolysis processes and generates cyanide ion, the cyano group in pesticide is directly carried out follow-up colour developing, it is not necessary to cyano group is converted into the hydrocyanic acid gas of severe toxicity, easy and simple to handle and safety and environmental protection.Owing to cyanide ion plays the part of the role of catalyst in chromogenic reaction, therefore along with the prolongation in response time, colour developing degree is deepened, it is possible to detects the cyano-containing pyrethroid pesticide of as little as GB limitation concentration, has higher sensitivity.Additionally, inspection card also has higher selectivity soon.By indicator is immobilized so that prepared fast inspection card has easy and simple to handle, it is easy to preserves, it is simple to the feature carried, can promote the use of.
Description
Technical field
The invention belongs to pyrethroid pesticide rapid detection technical field.Be specifically related to a kind of based on
The cyano-containing pyrethroid pesticide of chemical colour reaction principle examines the preparation of card and concrete application soon.
Background technology
Pyrethroid pesticide is to simulate natural pyrethrum, by an insecticides of synthetic.
Relative to other three major types insecticide, i.e. organophosphor, carbamate and organochlorine pesticide, intend deinsectization
The advantages such as pyrethrin pesticide has efficiently, low toxicity, are used by large-scale popularization the most.Especially containing cyanogen
Base pyrethroid pesticide, the application in fruit, growing vegetables is the most extensive.Scientific research table
Bright, the toxicity of cyano-containing pyrethroid pesticide has accumulative, and life-time service can cause poisoning thing
Part.Additionally, such pesticide is also considered to be environment incretion interferent and neurotoxic substance.Therefore,
Its residual on agricultural product is increasingly paid close attention to by people.
Accurate Sensitive Determination method currently for cyano-containing pyrethroid pesticide mainly uses
Large-scale instrument such as gas chromatogram, gas chromatography-mass spectrography etc., but instrument price is expensive, complex operation,
And reagent consumption is big, it is impossible to meet the demand of daily bread safe high flux inspection.In recent years,
The quick screening method to such pesticide of development mainly includes immunoassay and chemical staining method.So
And, immunoassay is required for every kind of cyano-containing pyrethroid pesticide and prepares corresponding antibody,
Technical sophistication, and relatively costly；Chemical staining method adds dense after generally utilizing the cyano group alkaline hydrolysis in pesticide
Acid makes it become severe toxicity gaseous hydrogen cyanic acid to carry out follow-up chromogenic reaction, not environmentally, dangerous, and aobvious
Color phenomenon is inconspicuous.Therefore, need a kind of simplicity of development badly, that sensitive and safety and environmental protection method realizes is right
The quick detection of cyano-containing pyrethroid pesticide.
Summary of the invention
It is an object of the invention to provide a kind of novel cyano-containing pyrethroid pesticide and examine card soon
Sheet, this card makes simple, easy to operate quickly, and the sensitiveest, be conducive to promoting the use of.
For achieving the above object, the technical solution used in the present invention is:
This soon inspection card immobilized have can be with cyano-containing pyrethroid pesticide rapid-action indicator
A；
Described indicator A is aromatic aldehyde compound, including benzaldehyde, to cyanobenzaldehyde, three
Hydroxy benzaldehyde, o-chlorobenzaldehyde, TMB, adjacent sulfonyloxy methyl benzaldehyde, adjacent nitre
Benzaldehyde, p-bromobenzaldehyde, dinitrobenzal-dehyde, paranitrobenzaldehyde, 3-nitro-4-chlorobenzene first
One or two or more kinds in aldehyde, cumaldehyde.
The material of described card is silica gel plate or filter paper.
20-100mg indicator A is joined 1mL silica gel sol gel solution or polymer solution
In, ultrasonic dissolution, take 1-3 μ L solution drop coating on card, be dried at room temperature for examining card soon.
Described indicator immobilized use silica gel sol gel solution or polymer solution, its preparation method is such as
Under:
1) preparation of silica gel sol gel solution: 1. by silicone agent, ethylene glycol monomethyl ether, propylene glycol
Methyl ether acetate, organic solvent, catalyst, surfactant and water are with 1:(2-4): (1-2):
(0.2-0.8): (0.1-0.8): (0.005-0.04): (0.5-1) volume ratio mixes, 40-70 DEG C
Stirring hydrolysis 2-6 hour, obtains silica gel sol gel solution A；Or 2. by silicone agent, ethylene glycol
Methyl ether, propylene glycol methyl ether acetate, catalyst, surfactant and water are with 1:(1-5): (1-4):
(0.1-1): (0.05-0.9): (0.5-1) volume ratio mixes, water at normal temperature solution 2-6 hour,
Obtain silica gel sol gel solution B；
2) preparation of polymer solution: 1. by polyvinyl alcohol, plasticizer, organic solvent and water with 1:(2
-6): (50-100): (30-70) mass ratio mixes, stirring reaction 1-3 hour under room temperature,
Polymer A solution；Or 2. by polyvinyl butyral resin, PEG-4000, plasticizer and organic molten
Agent is with 1:(2-6): (3-7): (80-120) mass ratio mixes, stirring reaction 1-3 under room temperature
Hour, obtain polymer B solution；Or 3. by polrvinyl chloride, plasticizer, Polyethylene Glycol and organic solvent
With 1:(2-6): (1-5): (50-100) mass ratio mixes, react 1-3 hour under room temperature,
Obtain polymer C solution.
Described silicone agent includes: tetramethoxy-silicane, tetraethoxysilane, methyl trimethoxy epoxide
Silane, MTES, normal octane triethoxysilane, (3-mercaptopropyi) trimethoxy silicon
Alkane, (3-aminopropyl) triethoxysilane, phenyl triethoxysilane, (3-chloropropyl) trimethoxy silicon
Alkane, one or two or more kinds in trim,ethylchlorosilane；
Described catalyst is the one or two in the hydrochloric acid of 0.1-1M, acetic acid or 0.05-0.5M sulphuric acid
More than Zhong；
Described surfactant is sodium lauryl sulphate, dodecylbenzene sodium sulfonate, cetyl three
Methyl bromide ammonium, polysorbas20, L7001, Span 60, triton x-100, Span 80 and carboxylic first
One or two or more kinds in base sodium cellulosate；
Described plasticizer is Plexol 201, phthalic acid two (2-ethyl hexyl) ester, O-phthalic
Acid di-n-octyl, trioctyl phosphate, one or two or more kinds in dimethyl phthalate；
Described organic solvent be ethanol, methanol, ether, acetonitrile, oxolane, dimethyl sulfoxide, three
One or two or more kinds in chloromethanes, hexamethylene, toluene.
Described fast inspection card is as follows to the detection process of cyano-containing pyrethroid pesticide: join with pure water
Make 0.8 1mL pesticide to 0.5 10ppm, add 30 55 μ L aqueous slkalis, add 0.5 1mL
Indicator B, places 2 10min after mixing, the above-mentioned mixed liquor taking 5 30 μ L drips to examine soon card
On sheet, the cyanide ion that immobilized indicator A can go out with pesticide alkaline hydrolysis reacts generation reproducibility chemical combination
Thing, and then reduction indicator B generation color compound, finally realize the fast of cyano-containing pyrethroid
Speed detection.
Described aqueous slkali is that hydroxide is dissolved in the ethanol containing volumetric concentration 50%-80% or second two
In the aqueous solution of alcohol methyl ether, concentration is in the range of 0.1 1M.
Described indicator B is dinitrobenzoic acid, o-dinitrobenzene, paradinitrobenzene, dinitro benzene
Formaldehyde, chloro triphenyltetrazolium chloride, iodo nitro tetrazolium, tetrazolium violet, tetrazolium blue, nitro tetrazolium blue
In any one, concentration is in the range of 0.02 0.5M.
Described cyano-containing pyrethroid pesticide include cypermethrin, decis, fenvalerate,
Fenpropathrin, cyfloxylate, lambda-cyhalothrin, Grenade (ICI)., fluorine fenvalerate, fluorine amine
One or two or more kinds in Cyano chrysanthemate.
Present invention have the advantage that
1. cyano-containing pyrethroid pesticide is examined card soon and is eliminated traditional inspection soon in such pesticide method
Need that pesticide cyano group alkaline hydrolysis is added concentrated acid and generate the process of severe toxicity gaseous hydrogen cyanic acid, and straight
Connect and cyanide ion is carried out follow-up chromogenic assay, be very environmental protection and safety；
2. the specific chemical between fast inspection card cyanide ion based on indicator and the generation of pesticide alkaline hydrolysis
Colour developing principle, therefore has higher selectivity when Multiple Pesticides coexists；And due to cyanogen root
Play catalytic action during ion and indicator reaction and make prolongation color product over time
Generation quantitative change many, thus improve detection sensitivity, therefore can balance according to actual needs
Relation between response time and sensitivity；
3. fast inspection card system is standby simple, cheap, easy to operate, owing to indicator is immobilized in porous
Material makes it easier to preserve, be easy to carry, it is adaptable to cyano-containing pyrethroid pesticide
Field quick detection.
Accompanying drawing illustrates:
Fig. 1 cyano-containing pyrethroid pesticide is examined card soon and is rung the gamma cyhalothrin of 2ppm
Should be over time；
Fig. 2 examines the card color response to the gamma cyhalothrin of variable concentrations soon；
Fig. 3 examines the selectivity of card soon；
Fig. 4 examine soon card to various cyano-containing pyrethroid pesticides GB limitation concentration under sound
Should.
Detailed description of the invention
Embodiment 1.
The preparation of card examined soon by cyano-containing pyrethroid pesticide silica gel plate: weigh 30mg to cyano group
Benzaldehyde in 1mL polymer B (polyvinyl butyral resin, PEG-4000, trioctyl phosphate and
Ethanol, with 1:2:5:100, stirs 2 hours under room temperature, obtains polymer B) in, ultrasonic dissolution,
Then drawing the 3 above-mentioned solution of μ L with liquid-transfering gun, drop coating, on silica gel plate card, prepares cyano-containing
Pyrethroid pesticide examines card soon.
Embodiment 2.
Cyano-containing pyrethroid pesticide paper substrate examines the preparation of card soon: weigh 50mg p-nitrophenyl
Formaldehyde is in 1mL silica gel sol gel solution A (tetraethoxysilane: ethylene glycol monomethyl ether: propylene glycol first
Ether acetate: chloroform: 1M HCl: Span 60: water is with 1:3:3:0.5:0.4:0.005:
1 volume ratio mixing, 60 DEG C hydrolyze 5 hours, obtain silica gel sol gel solution A) in, ultrasonic dissolution,
Then drawing the 1 above-mentioned solution of μ L with liquid-transfering gun, drop coating, on paper substrate card, prepares cyano-containing and intends
Card examined soon by cinerins pesticide.
Embodiment 3.
Investigate fast inspection card prepared in embodiment 1 in detection cyano-containing pyrethroid pesticide mistake
In journey, color is over time.With gamma cyhalothrin as representative, preparation 1mL concentration is 2ppm
Gamma cyhalothrin aqueous solution.Adding 50 μ L concentration in this solution is the sodium hydroxide of 0.5M
Solution (solvent is the ethanol water of 60%), adds the chloro triphen that 0.5mL concentration is 0.2M
Base tetrazole solution (solvent is water), 5min is placed in mixing.Take the 10 above-mentioned solution of μ L and drop in card
Immobilized indicator central authorities, utilize mobile phone camera function to remember indicator color over time
Record, respectively 0,5,10,20min time fast inspection card is taken pictures, as shown in Figure 1.Along with reaction
The prolongation of time, card color is gradually deepened, and can see that when 10min obvious color changes,
Ensureing higher sensitivity for shortening detection process, subsequent experimental all uses 10min as reaction simultaneously
The record time.
Embodiment 4.
Investigate the fast inspection card response to variable concentrations gamma cyhalothrin prepared in embodiment 2.
Preparation 1mL concentration is the gamma cyhalothrin aqueous solution of 2ppm and 5ppm respectively.And with 1mL
Pure water, as comparison, is separately added into the sodium hydroxide that 50 μ L concentration are 0.5M molten in three kinds of solution
Liquid (solvent is the ethanol water of 60%), then it is separately added into the chloro three that 0.5mL concentration is 0.1M
Phenyl tetrazole solution (solvent is water), 10min is placed in mixing.Take the 20 above-mentioned solution of μ L respectively to drip
In the indicator central authorities that three fast inspection cards are immobilized, three cards of mobile phone camera function record are utilized to put
Put color during 10min, as shown in Figure 2.Visible, the concentration of gamma cyhalothrin is the biggest, card
Sheet color is the deepest.Therefore, available this examines card by shade soon to cyano-containing pyrethroid
Class pesticide carries out half-quantitative detection.
Embodiment 5.
Investigate the fast inspection card selection to cyano-containing pyrethroid pesticide prepared in embodiment 1
Property.It is known that agricultural insecticide class pesticide mainly includes four big class, i.e. organic phosphates, amino first
Esters of gallic acid, pyrethroid and organochlorine class.In recent years, some emerging organic nitrogen sulfur classes etc. are low
Poison insecticide occupies the most rapidly market.In the middle of the present embodiment, we select above-mentioned a few class to kill respectively
The representative products of worm agent has carried out the selectivity experiment of fast inspection card.Preparation 1mL concentration is 5 respectively
The chlopyrifos (organic phosphates) of ppm, Mobucin (carbamates), drinox (organochlorine class),
Kill snout moth's larva list (organic nitrogen sulfur class) and decis (pyrethroid) aqueous solution, still with 1mL
Pure water is comparison.Being separately added into 50 μ L concentration in above-mentioned comparison and the pesticide solution is the hydrogen of 0.5M
Sodium hydroxide solution (solvent is the ethanol water of 60%), then to be separately added into 0.5mL concentration be 0.02M
Chloro triphenyltetrazolium chloride solution (solvent is water), mixing place 5min.Take respectively on 10 μ L
State solution and drop in the indicator central authorities that fast inspection card is immobilized, utilize the mobile phone camera each card of function record to exist
Place color during 10min, as shown in Figure 3.Result shows except the card of detection decis has
Significantly outside color change, other kinds of pesticide all will not make card produce color change, and institute is described
The fast inspection card of preparation has higher selectivity.
Embodiment 6.
Investigate fast inspection card prepared in embodiment 1 various cyano-containing pyrethroid pesticides are existed
Response condition under GB limitation concentration.Cypermethrin (5 under preparation 1mL GB limitation concentration respectively
Ppm), Fenpropathrin (1ppm), fenvalerate (3ppm), gamma cyhalothrin (2ppm)
With taufluvalinate (0.5ppm) aqueous solution, compare with 1mL pure water.To above-mentioned comparison and
(solvent is the second of 60% to be separately added into the sodium hydroxide solution that 50 μ L concentration are 0.5M in the pesticide solution
Alcohol-water solution), then it is (molten to be separately added into the chloro triphenyltetrazolium chloride solution that 0.5mL concentration is 0.02M
Agent is water), 5min is placed in mixing.Take the 10 above-mentioned solution of μ L respectively and drop in the finger that fast inspection card is immobilized
Show agent central authorities, utilize the mobile phone camera each card of the function record color when placing 10min, such as Fig. 4
Shown in.Visible, fast inspection card is equal to the cyano-containing pyrethroid pesticide under each GB limitation concentration
Can produce the color response that naked eyes can be distinguished, prepared card is applicable to cyano-containing pyrethroid agriculture
The field quick detection of medicine.
Claims (9)
1. a cyano-containing pyrethroid pesticide examine card soon, it is characterised in that: this examines card soon
Sheet is immobilized, and have can be with cyano-containing pyrethroid pesticide rapid-action indicator A；
Described indicator A is aromatic aldehyde compound, including benzaldehyde, to cyanobenzaldehyde, three
Hydroxy benzaldehyde, o-chlorobenzaldehyde, TMB, adjacent sulfonyloxy methyl benzaldehyde, adjacent nitre
Benzaldehyde, p-bromobenzaldehyde, dinitrobenzal-dehyde, paranitrobenzaldehyde, 3-nitro-4-chlorobenzene first
One or two or more kinds in aldehyde, cumaldehyde.
Fast inspection card the most according to claim 1, it is characterised in that:
The material of described card is silica gel plate or filter paper.
3. the fast preparation method examining card described in a claim 1 or 2, it is characterised in that: by 20
-100mg indicator A joins in 1mL silica gel sol gel solution or polymer solution, ultrasonic
Dissolve, take 1-3 μ L solution drop coating on card, be dried at room temperature for examining card soon.
Examine the preparation method of card the soonest, it is characterised in that: described instruction
Agent immobilized use silica gel sol gel solution or polymer solution, its preparation method is as follows:
1) preparation of silica gel sol gel solution: 1. by silicone agent, ethylene glycol monomethyl ether, propylene glycol
Methyl ether acetate, organic solvent, catalyst, surfactant and water are with 1:(2-4): (1-2):
(0.2-0.8): (0.1-0.8): (0.005-0.04): (0.5-1) volume ratio mixes, 40-70 DEG C
Stirring hydrolysis 2-6 hour, obtains silica gel sol gel solution A；Or 2. by silicone agent, ethylene glycol
Methyl ether, propylene glycol methyl ether acetate, catalyst, surfactant and water are with 1:(1-5): (1-4):
(0.1-1): (0.05-0.9): (0.5-1) volume ratio mixes, water at normal temperature solution 2-6 hour,
Obtain silica gel sol gel solution B；
2) preparation of polymer solution: 1. by polyvinyl alcohol, plasticizer, organic solvent and water with 1:(2
-6): (50-100): (30-70) mass ratio mixes, stirring reaction 1-3 hour under room temperature,
Polymer A solution；Or 2. by polyvinyl butyral resin, PEG-4000, plasticizer and organic molten
Agent is with 1:(2-6): (3-7): (80-120) mass ratio mixes, stirring reaction 1-3 under room temperature
Hour, obtain polymer B solution；Or 3. by polrvinyl chloride, plasticizer, Polyethylene Glycol and organic solvent
With 1:(2-6): (1-5): (50-100) mass ratio mixes, react 1-3 hour under room temperature,
Obtain polymer C solution.
Preparation method the most according to claim 3, it is characterised in that:
Described silicone agent includes: tetramethoxy-silicane, tetraethoxysilane, methyl trimethoxy epoxide
Silane, MTES, normal octane triethoxysilane, (3-mercaptopropyi) trimethoxy silicon
Alkane, (3-aminopropyl) triethoxysilane, phenyl triethoxysilane, (3-chloropropyl) trimethoxy silicon
Alkane, one or two or more kinds in trim,ethylchlorosilane；
Described catalyst is the one or two in the hydrochloric acid of 0.1-1M, acetic acid or 0.05-0.5M sulphuric acid
More than Zhong；
Described surfactant is sodium lauryl sulphate, dodecylbenzene sodium sulfonate, cetyl three
Methyl bromide ammonium, polysorbas20, L7001, Span 60, triton x-100, Span 80 and carboxylic first
One or two or more kinds in base sodium cellulosate；
Described plasticizer is Plexol 201, phthalic acid two (2-ethyl hexyl) ester, O-phthalic
Acid di-n-octyl, trioctyl phosphate, one or two or more kinds in dimethyl phthalate；
Described organic solvent be ethanol, methanol, ether, acetonitrile, oxolane, dimethyl sulfoxide, three
One or two or more kinds in chloromethanes, hexamethylene, toluene.
6. the fast application examining card described in a claim 1 or 2, it is characterised in that: described fast inspection
Card is as follows to the detection process of cyano-containing pyrethroid pesticide: prepare 0.8 1mL with pure water
Pesticide, to 0.5 10ppm, adds 30 55 μ L aqueous slkalis, adds 0.5 1mL indicator B,
Placing 2 10min after mixing, the above-mentioned mixed liquor taking 5 30 μ L drips to examine on card soon, immobilized
The cyanide ion that can go out with pesticide alkaline hydrolysis of indicator A react generation reproducibility compound, and then also
Former indicator B generates color compound, finally realizes the quick detection of cyano-containing pyrethroid.
Application the most according to claim 6, it is characterised in that:
Described aqueous slkali is that hydroxide is dissolved in the ethanol containing volumetric concentration 50%-80% or second two
In the aqueous solution of alcohol methyl ether, concentration is in the range of 0.1 1M.
Application the most according to claim 6, it is characterised in that:
Described indicator B is dinitrobenzoic acid, o-dinitrobenzene, paradinitrobenzene, dinitro benzene
Formaldehyde, chloro triphenyltetrazolium chloride, iodo nitro tetrazolium, tetrazolium violet, tetrazolium blue, nitro tetrazolium blue
In any one, concentration is in the range of 0.02 0.5M.
Application the most according to claim 6, it is characterised in that: described cyano-containing pyrethroid
Class pesticide includes cypermethrin, decis, fenvalerate, Fenpropathrin, cyfloxylate, chlorine
One or two or more kinds in flucythrinate, Grenade (ICI)., fluorine fenvalerate, taufluvalinate.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610251288.9A CN106226292B (en) | 2016-04-21 | 2016-04-21 | A kind of fast inspection card of cyano-containing pyrethroid pesticide and preparation and application |
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|---|---|---|---|
| CN201610251288.9A CN106226292B (en) | 2016-04-21 | 2016-04-21 | A kind of fast inspection card of cyano-containing pyrethroid pesticide and preparation and application |
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| CN106226292B CN106226292B (en) | 2018-07-03 |
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