CN106198508A - A kind of high sensitivity quickly detects the method containing heavy metal class pesticide - Google Patents
A kind of high sensitivity quickly detects the method containing heavy metal class pesticide Download PDFInfo
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Abstract
The present invention has developed a kind of quick detection method containing heavy metal class pesticide based on the principle that the strong chelation between metal-chelating indicator and heavy metal makes indicator produce color change.Its special colour developing principle makes the method be only applicable to, containing heavy metal class pesticide, have higher selectivity.And by by immobilized for indicator on porous material, pesticide constantly can occur to answer with indicator to utilize enrichment mode, thus is greatly improved detection sensitivity.Additionally, there is good linear relationship between the change of indicator color and the concentration containing heavy metal class pesticide, such pesticide can be carried out detection by quantitative.This method is easy and simple to handle, and sensor is cheap, is suitable as supplementing and promoting the use of of existing pesticide residue detection method.
Description
Technical field
The invention belongs to Pesticides Testing technical field.It is specifically related to one and utilizes colorimetric sensor, pass through
Enrichment, reaches quick, high sensitivity and the high selective enumeration method method containing heavy metal class pesticide.
Background technology
In world wide, the growth of population promotes the mankind day by day to increase severely the demand of grain, in order to improve grain
Food yield, the use of pesticide is essential.In the market Pesticidal products kind mainly include insecticide,
Herbicide and antibacterial.Wherein, the demand of antibacterial constantly rises, and speedup is very fast.Have been reported that
Point out, the kind that antibacterial demand in 2015 is bigger include copper fungicide, for gloomy class, good fortune U.S. class,
Bravo, carbendazim, tricyclazole etc., first three class in these antibacterial all contains heavy metal element.
The brought problem that is widely used containing heavy metal class pesticide includes two aspects.On the one hand, by
In the character unique containing heavy metal class pesticide so that it is the most at that time can generation with other class mixed pesticides
Learn reaction, thus affect drug effect and even produce poisoning, cause crops harvest to decline.On the other hand,
Owing to the mechanism of action of such pesticide is that metal can destroy the cellularity of thalline, make tropina
Matter solidifies, and its residual on food can be finally by human intake, so that human body protein generation can not
The degeneration reversed, disturbs normal physiological function, produces toxic action.Additionally, such pesticide also can be
Water body, discharges heavy metal, works the mischief water body and geobiont, cause ecology in the environment such as soil
Ecological deterioration.
By reducing environment and the health risk that heavy metal class pesticide is brought, it is necessary to residual to such pesticide
Stay and be estimated.But the fast detecting method of pesticide residues the most on the market is limited only to organic phosphates and ammonia
Carbamate class pesticide, not for the quick detection means of such pesticide, therefore needs development one badly
Plant short-cut method highly sensitive, visual to realize the real time monitoring containing heavy metal pesticide residue.
Summary of the invention
It is an object of the invention to provide the fast and convenient detection of a kind of high sensitivity containing heavy metal class pesticide
Method, supplements for the existing fast detecting method of pesticide residues.
For achieving the above object, the technical solution used in the present invention is:
On porous material, sensor is prepared by immobilized for indicator；
Detection process: by sensor and Pesticide Exposure, by indicator and containing in heavy metal class pesticide
Chelation between heavy metal makes the indicator on sensor produce color reaction, and passes through sensor
Quantitative pesticide is enriched with the color change intensity improving indicator, then utilizes imaging device to adopt
Image before and after collection indicator reaction, the color extracting wherein red, green, blue (RGB) three passages becomes
Change value；Then formula is utilizedIt is calculated sensor to react with pesticide
Color changing value ED front and back；
1) the heavy metal pesticide containing known variable concentrations is operated according to above-mentioned detection process, point
Not with concentration, color changing value ED for transverse and longitudinal coordinate, build the class pesticide Han heavy metal corresponding dense
Degree gradient standard curve；
2) operate according to above-mentioned detection process containing heavy metal class pesticide to be detected, it is thus achieved that color becomes
Change value ED, obtains the levels of its correspondence by standard curve.
The preparation process of described sensor is: takes 0.5-5mg indicator and joins 1m silica gel colloidal sol
In gel solution or polymer solution, ultrasonic dissolution, take 1-3 μ L solution drop coating on porous material,
Drying at room temperature under nitrogen protection,
Described silica gel sol gel solution or polymer solution, its preparation method is as follows:
1) synthesis of silica gel collosol and gel: 1. by silicone agent, ethylene glycol monomethyl ether, propylene glycol monomethyl 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, 30-60 DEG C of stirring
Hydrolyze 4-10 hour, obtain silica gel sol gel solution A；Or 2. by silicone agent, ethylene glycol first
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, 15-40 DEG C of stirring hydrolysis 20-30
Hour, obtain silica gel sol gel solution B；
2) synthesis of polymer: 1. by polyvinyl alcohol, plasticizer, organic solvent and water with 1:(2-6):
(50-100): (30-70) mass ratio mixes, stirring reaction 0.5-5 hour at 15-40 DEG C,
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, stir reaction 2 at 15-40 DEG C
-4 hours, obtain polymer B solution；Or 3. by polrvinyl chloride, plasticizer, Polyethylene Glycol and organic
Solvent is with 1:(2-6): (1-5): (50-100) mass ratio mixes, react 2-at 15-40 DEG C
4 hours, obtain polymer C solution；
Described indicator is metal-chelating indicator, including aminophenazone, alizarin, 1,2-hexamethylene two
Ketone dioxime, chlorophosphonazo Ⅲ, dithizone, 2,2'-bipyridyl, 1-pyridylazo-beta naphthal, chromotropic acid
One or two or more kinds in 2B, diphenyl carbazone, murexide, Saldox.；
Described porous material is porous filter paper, nitric acid-acetic acid composite fibre resin molding, Kynoar
Film or poly tetrafluoroethylene.
Described silicone agent includes: tetramethoxy-silicane, tetraethoxysilane, methyl trimethoxy oxygen
Base silane, MTES, normal octane triethoxysilane, (3-mercaptopropyi) trimethoxy
Silane, (3-aminopropyl) triethoxysilane, phenyl triethoxysilane, (3-chloropropyl) trimethoxy
One or two or more kinds in silane, trim,ethylchlorosilane；Catalyst be 0.05-1.5M hydrochloric acid,
One or two or more kinds in acetic acid, sulphuric acid or nitric acid；Surfactant be sodium lauryl sulphate,
Dodecylbenzene sodium sulfonate, cetyl trimethylammonium bromide, polysorbas20, L7001, Span 60,
One or two or more kinds in triton x-100, Span 80 and sodium carboxymethyl cellulose.
Organic solvent used in described silica gel sol gel solution or polymer solution building-up process is first
Alcohol, ethanol, ether, acetonitrile, acetone, oxolane, dimethyl sulfoxide, chloroform, hexamethylene,
One or two or more kinds in toluene.
Described plasticizer is Plexol 201, phthalic acid two (2-ethyl hexyl) ester, O-phthalic
One or two or more kinds in acid di-n-octyl, trioctyl phosphate, dimethyl phthalate.
The described class pesticide containing heavy metal include copper sulfate, Copper hydrate, Red copper oxide, copper oxychloride,
Bordeaux mixture, Cupravit, network ammonia copper, copper acetate, copper 8-hydroxyquinolinate, Thiodiazole-copper, nonylphenolsulfonate copper, copper rosinate,
Zinc thiazole, zineb, maneb, Mancozeb, Propineb, ferric dimethyldithiocarbamate, ziram, maneb
One or two or more kinds in copper, Carbatene, azacyclotin, fenbutatin oxide, mercuric chloride.
Described imaging device is CCD, digital camera, camera mobile phone or scanner.
The described class Pesticides Testing process containing heavy metal is as follows: the preparation pure water containing heavy metal class pesticide is molten
Liquid 0.1-10mg/L, takes 5-50 μ L and drips on sensor, immobilized indicator can with in pesticide
Heavy metal generation chelatropic reaction so that the color of indicator changes, unnecessary solution is through many
Porous materials, is absorbed by pad absorbent filter below sensor；Pesticide liquid to be measured is dripped constantly
During, utilize the capillarity of absorbent filter to realize the enrichment to pesticide, so that color change
Strengthen, improve the detection sensitivity of detector；After sample test process, imaging device is utilized to adopt
Image before and after collection sensor response, and utilizeThe given zone that color is homogeneous selected by software
Territory, tries to achieve the color average RGB value of its correspondence, by image digitazation intuitively, and carries out subtractive；
The standard concentration curve containing heavy metal class pesticide is built with Concentraton gradient by color changing value.
Present invention have the advantage that
1. provide a kind of for the New Method for Rapid containing heavy metal class pesticide, examine for existing
The pesticide surveyed is supplemented；
2. this method by by immobilized for indicator on porous material, it is possible to by enrichment promote detection spirit
Sensitivity；
3. this method utilizes indicator and containing the strong chelation between the heavy metal in heavy metal class pesticide
Generation color changes, and therefore such pesticide has higher when coexisting with other kind pesticide
Selectivity；
4. this method is with low cost, easy and simple to handle, and prepared sensor is easy to carry, it is adaptable to existing
Field quickly detection.
Accompanying drawing illustrates:
Fig. 1 is the prepared selectivity figure containing metal class pesticide sensor；
Concentration effect (enrichment volume unit the is μ L) figure of Fig. 2 (a) sensor, Fig. 2 (b) sensor is surveyed
Determine the standard concentration curve figure of ziram.
Detailed description of the invention
Embodiment 1.
Preparation containing heavy metal class pesticide colorimetric sensor: weigh the 1-pyridylazo-beta naphthal of 2mg in
0.5mL silica gel collosol and gel A (tetramethoxy-silicane: ethylene glycol monomethyl ether: propylene glycol methyl ether acetate:
Oxolane: 0.05M sulphuric acid: polysorbas20: water is with 1:3:2:0.5:0.8:0.03:0.6 volume
Than mixing, 50 DEG C hydrolyze 8 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 is in the porous filter paper of aperture 0.22 μm, and nitrogen is protected
I.e. it is prepared as after protecting lower drying at room temperature containing heavy metal class pesticide sensor.
Embodiment 2.
The selectivity to variety classes pesticide of the class pesticide sensor containing heavy metal: utilize flat bed scanner to remember
Record the image before and after sensor reacts with variety classes pesticide.The color of image before and after reaction is usedSoftware digital, extracts RGB (RGB) channel value, and to each logical before and after reaction
Road color data carries out subtractive, obtains each passage color changing value Δ R, Δ G, Δ B, then utilizes public affairs
FormulaIt is calculated the face before and after sensor reacts with variety classes pesticide
Color changing value ED, as shown in Figure 1.It will be seen from figure 1 that sensor to 1ppm containing heavy metal
Class pesticide is (with Propineb, Carbatene, ziram, maneb, Mancozeb, zineb, hydrogen-oxygen
Change copper, Cupravit, Red copper oxide, copper 8-hydroxyquinolinate, zinc thiazole are representative) there is obvious color response,
And other series bactericidal agents are included Bravo, tolelofos-methyl, insecticide includes that organic phosphates (is poisoned with poison
Ticks), carbamates (Mobucin), pyrethroid (cypermethrin) and herbicide such as cyanogen
Even if fluorine grass ester also will not produce the change of significant color under the concentration of 5ppm, prepared by explanation
Sensor has high selectivity to the class pesticide containing heavy metal, it is adaptable to the actual sample that Multiple Pesticides coexists
In containing the detection of heavy metal class pesticide.
Embodiment 3.
The concentration effect of sensor prepared in embodiment 1 and it is to responding containing heavy metal class pesticide
Concentration standard curve: with containing the ziram in heavy metal class pesticide as representative, result is as shown in Figure 2.
During from Fig. 2 (a) it can be seen that the ziram aqueous solution containing 1ppm is added drop-wise to sensor, along with dropping
The volume of pesticide constantly increases, and sensor colors change gradually strengthens, and illustrates by enrichment, Ke Yi great
The big detection sensitivity promoting sensor.For being easy to operate quickly, the pesticide solution taking 400 μ L is made
Enrichment volume in testing for Criterion concentration curve.Compound concentration is 0.5,1,1.5,2,2.5 respectively
The ziram aqueous solution of ppm.Respectively take the 400 above-mentioned solution of μ L to be added drop-wise to respectively on sensor, treat solution
After being blotted by pad absorbent filter below sensor, utilize flat bed scanner record image, with enrichment
The sensor of 400 μ L pure water is image before reaction, and the sensor being enriched with each concentration ziram solution is anti-
Should image afterwards, will imagery exploitation before and after reactionSoftware digital, extracts RGB (RGB)
Channel value, and each passage color data before and after reaction is carried out subtractive, obtain each passage color changing value
Δ R, Δ G, Δ B, then utilize formulaIt is calculated sensor with each
Color changing value ED before and after concentration ziram solution reaction, as shown in Fig. 2 (b).Result shows, with
The increase of ziram concentration, sensor colors change strengthens.By dense with ziram for color changing value ED
Degree does figure, obtains the standard curve containing heavy metal class pesticide sensor detection ziram pesticide,
Y=28.82x+15.44 (R2=0.9981), it is seen then that in the concentration range internal indicator face of 0.5～2.5ppm
There is between complexion changed and ziram concentration good linear relationship, therefore can utilize this concentration standard
Ziram concentration in sample is quantitative determined by curve.
Claims (8)
1. a high sensitivity quickly detects the method containing heavy metal class pesticide, it is characterised in that:
On porous material, sensor is prepared by immobilized for indicator；
Detection process: by sensor and Pesticide Exposure, the indicator on sensor is made to produce color reaction by indicator and containing the chelation between the heavy metal in heavy metal class pesticide, and by sensor quantitative pesticide is enriched with the color change intensity improving indicator, then utilize imaging device to gather image before and after indicator reaction, extract the color changing value of wherein red, green, blue (RGB) three passages；Then formula is utilizedIt is calculated the color changing value ED before and after sensor reacts with pesticide；
1) the heavy metal pesticide containing known variable concentrations is operated according to above-mentioned detection process, respectively with concentration, color changing value ED for transverse and longitudinal coordinate, build the corresponding Concentraton gradient standard curve in heavy metal class pesticide；
2) operate according to above-mentioned detection process containing heavy metal class pesticide to be detected, it is thus achieved that color changing value ED, obtained the levels of its correspondence by standard curve.
Detection method the most according to claim 1; it is characterized in that: the preparation process of described sensor is: take 0.5-5mg indicator and join in 1mL silica gel sol gel solution or polymer solution; ultrasonic dissolution; take 1-3 μ L solution drop coating on porous material; drying at room temperature under nitrogen protection
Described silica gel sol gel solution or polymer solution, its preparation method is as follows:
1) synthesis of silica gel collosol and gel: 1. by silicone agent, ethylene glycol monomethyl ether, propylene glycol methyl ether acetate, organic solvent, catalyst, surfactant and water with 1:(2-4): (1-2): (0.2-0.8): (0.1-0.8): (0.005-0.04): (0.5-1) volume ratio mixes, 30-60 DEG C of stirring hydrolyzes 4-10 hour, obtains silica gel sol gel solution A；Or 2. by silicone agent, ethylene glycol monomethyl ether, propylene glycol methyl ether acetate, catalyst, surfactant and water with 1:(1-5): (1-4): (0.1-1): (0.05-0.9): (0.5-1) volume ratio mix, 15-40 DEG C of stirring hydrolyzes 20-30 hour, obtains silica gel sol gel solution B；
2) synthesis of polymer: 1. by polyvinyl alcohol, plasticizer, organic solvent and water with 1:(2-6): (50-100): (30-70) mass ratio mixes, at 15-40 DEG C, stirring reaction 0.5-5 hour, obtains polymer A solution；Or 2. by polyvinyl butyral resin, PEG-4000, plasticizer and organic solvent with 1:(2-6): (3-7): (80-120) mass ratio mix, at 15-40 DEG C, stirring reaction 2-4 hour, obtains polymer B solution；Or 3. by polrvinyl chloride, plasticizer, Polyethylene Glycol and organic solvent with 1:(2-6): (1-5): (50-100) mass ratio mix, at 15-40 DEG C react 2-4 hour, obtain polymer C solution；
Described indicator is metal-chelating indicator, including aminophenazone, alizarin, 1,2-cyclohexanedionedioxime, chlorophosphonazo Ⅲ, dithizone, 2, one or two or more kinds in 2'-bipyridyl, 1-pyridylazo-beta naphthal, Chromotrope 2B, diphenyl carbazone, murexide, Saldox.；
Described porous material is porous filter paper, nitric acid-acetic acid composite fibre resin molding, polyvinylidene fluoride film or poly tetrafluoroethylene.
Preparation method the most according to claim 2, it is characterised in that: described silicone agent includes: one or two or more kinds in tetramethoxy-silicane, tetraethoxysilane, MTMS, MTES, normal octane triethoxysilane, (3-mercaptopropyi) trimethoxy silane, (3-aminopropyl) triethoxysilane, phenyl triethoxysilane, (3-chloropropyl) trimethoxy silane, trim,ethylchlorosilane；Catalyst is one or two or more kinds in the hydrochloric acid of 0.05-1.5M, acetic acid, sulphuric acid or nitric acid；Surfactant is one or two or more kinds in sodium lauryl sulphate, dodecylbenzene sodium sulfonate, cetyl trimethylammonium bromide, polysorbas20, L7001, Span 60, triton x-100, Span 80 and sodium carboxymethyl cellulose.
Preparation method the most according to claim 2, it is characterised in that: organic solvent used in described silica gel sol gel solution or polymer solution building-up process is one or two or more kinds in methanol, ethanol, ether, acetonitrile, acetone, oxolane, dimethyl sulfoxide, chloroform, hexamethylene, toluene.
Preparation method the most according to claim 2, it is characterised in that: described plasticizer is one or two or more kinds in Plexol 201, phthalic acid two (2-ethyl hexyl) ester, dinoctyl phthalate, trioctyl phosphate, dimethyl phthalate.
Detection method the most according to claim 1, it is characterised in that: the described class pesticide containing heavy metal includes one or two or more kinds in copper sulfate, Copper hydrate, Red copper oxide, copper oxychloride, Bordeaux mixture, Cupravit, network ammonia copper, copper acetate, copper 8-hydroxyquinolinate, Thiodiazole-copper, nonylphenolsulfonate copper, copper rosinate, zinc thiazole, zineb, maneb, Mancozeb, Propineb, ferric dimethyldithiocarbamate, ziram, mancopper, Carbatene, azacyclotin, fenbutatin oxide, mercuric chloride.
Detection method the most according to claim 1, it is characterised in that: described imaging device is CCD, digital camera, camera mobile phone or scanner.
Detection method the most according to claim 1, it is characterized in that: the described class Pesticides Testing process containing heavy metal is as follows: the preparation pure water solution 0.1-10mg/L containing heavy metal class pesticide, take 5-50 μ L and drip on sensor, immobilized indicator can be with the heavy metal generation chelatropic reaction in pesticide so that the color of indicator changes, unnecessary solution passes through porous material, is absorbed by pad absorbent filter below sensor；During constantly dripping pesticide liquid to be measured, utilize the capillarity of absorbent filter to realize the enrichment to pesticide, so that color change strengthens, improve the detection sensitivity of detector；After sample test process, the image before and after utilizing imaging device to gather sensor response, and utilizeThe specific region that color is homogeneous selected by software, tries to achieve the color average RGB value of its correspondence, by image digitazation intuitively, and carries out subtractive；The standard concentration curve containing heavy metal class pesticide is built with Concentraton gradient by color changing value.
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| CN109900685A (en) * | 2017-12-07 | 2019-06-18 | 中国科学院宁波材料技术与工程研究所 | Sensor array and the preparation method and application thereof for detecting pesticide residue |
| CN109900685B (en) * | 2017-12-07 | 2021-12-17 | 中国科学院宁波材料技术与工程研究所 | Array sensor for detecting pesticide residues and preparation method and application thereof |
| CN108181304B (en) * | 2017-12-29 | 2021-02-26 | 漳州职业技术学院 | Method for detecting concentration of mercury ions in water |
| CN108181304A (en) * | 2017-12-29 | 2018-06-19 | 漳州职业技术学院 | The detection method of ion concentration of mercury in a kind of water |
| CN109738566A (en) * | 2019-02-27 | 2019-05-10 | 贵州健安德科技有限公司 | A method of utilizing copper 8-hydroxyquinolinate in UPLC-MS/MS method detection water |
| CN109738566B (en) * | 2019-02-27 | 2021-04-02 | 贵州健安德科技有限公司 | Method for detecting oxine-copper in water by using UPLC-MS/MS method |
| CN112113935A (en) * | 2019-06-19 | 2020-12-22 | 中国科学院大连化学物理研究所 | Fermat pesticide detection method based on manganese-containing inorganic-organic hybrid material |
| CN112113935B (en) * | 2019-06-19 | 2021-11-16 | 中国科学院大连化学物理研究所 | Fermat pesticide detection method based on manganese-containing inorganic-organic hybrid material |
| CN110542680B (en) * | 2019-07-16 | 2021-07-20 | 华南理工大学 | Portable wastewater COD detection device based on 3D printing paper base and manufacturing and measuring method |
| CN110542680A (en) * | 2019-07-16 | 2019-12-06 | 华南理工大学 | Portable wastewater COD detection device based on 3D printing paper base and manufacturing and measuring method |
| CN111175229A (en) * | 2020-01-19 | 2020-05-19 | 厦门大学 | In-situ detection device for dissolved Fe (II) and S (-II) in sediment section pore water and application thereof |
| CN112986476A (en) * | 2021-02-06 | 2021-06-18 | 广西思浦林科技有限公司 | Method for measuring residual quantity of cuaminosulfate in vegetables and fruits |
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